[go: up one dir, main page]

WO2025259841A1 - Crystalline forms of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]jmethyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one - Google Patents

Crystalline forms of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]jmethyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one

Info

Publication number
WO2025259841A1
WO2025259841A1 PCT/US2025/033293 US2025033293W WO2025259841A1 WO 2025259841 A1 WO2025259841 A1 WO 2025259841A1 US 2025033293 W US2025033293 W US 2025033293W WO 2025259841 A1 WO2025259841 A1 WO 2025259841A1
Authority
WO
WIPO (PCT)
Prior art keywords
salt
compound
powder diffraction
ray powder
crystalline form
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
PCT/US2025/033293
Other languages
French (fr)
Inventor
Dietrich Steinhuebel
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nested Therapeutics Inc
Original Assignee
Nested Therapeutics Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Nested Therapeutics Inc filed Critical Nested Therapeutics Inc
Publication of WO2025259841A1 publication Critical patent/WO2025259841A1/en
Pending legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D405/00—Heterocyclic compounds containing both one or more hetero rings having oxygen atoms as the only ring hetero atoms, and one or more rings having nitrogen as the only ring hetero atom
    • C07D405/02—Heterocyclic compounds containing both one or more hetero rings having oxygen atoms as the only ring hetero atoms, and one or more rings having nitrogen as the only ring hetero atom containing two hetero rings
    • C07D405/12—Heterocyclic compounds containing both one or more hetero rings having oxygen atoms as the only ring hetero atoms, and one or more rings having nitrogen as the only ring hetero atom containing two hetero rings linked by a chain containing hetero atoms as chain links
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P35/00—Antineoplastic agents
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C211/00—Compounds containing amino groups bound to a carbon skeleton
    • C07C211/01—Compounds containing amino groups bound to a carbon skeleton having amino groups bound to acyclic carbon atoms
    • C07C211/02—Compounds containing amino groups bound to a carbon skeleton having amino groups bound to acyclic carbon atoms of an acyclic saturated carbon skeleton
    • C07C211/03—Monoamines
    • C07C211/05—Mono-, di- or tri-ethylamine
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C215/00—Compounds containing amino and hydroxy groups bound to the same carbon skeleton
    • C07C215/02—Compounds containing amino and hydroxy groups bound to the same carbon skeleton having hydroxy groups and amino groups bound to acyclic carbon atoms of the same carbon skeleton
    • C07C215/40—Compounds containing amino and hydroxy groups bound to the same carbon skeleton having hydroxy groups and amino groups bound to acyclic carbon atoms of the same carbon skeleton with quaternised nitrogen atoms bound to carbon atoms of the carbon skeleton
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C309/00—Sulfonic acids; Halides, esters, or anhydrides thereof
    • C07C309/01—Sulfonic acids
    • C07C309/02—Sulfonic acids having sulfo groups bound to acyclic carbon atoms
    • C07C309/03—Sulfonic acids having sulfo groups bound to acyclic carbon atoms of an acyclic saturated carbon skeleton
    • C07C309/05—Sulfonic acids having sulfo groups bound to acyclic carbon atoms of an acyclic saturated carbon skeleton containing at least two sulfo groups bound to the carbon skeleton
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C309/00—Sulfonic acids; Halides, esters, or anhydrides thereof
    • C07C309/01—Sulfonic acids
    • C07C309/28—Sulfonic acids having sulfo groups bound to carbon atoms of six-membered aromatic rings of a carbon skeleton
    • C07C309/33—Sulfonic acids having sulfo groups bound to carbon atoms of six-membered aromatic rings of a carbon skeleton of six-membered aromatic rings being part of condensed ring systems
    • C07C309/34—Sulfonic acids having sulfo groups bound to carbon atoms of six-membered aromatic rings of a carbon skeleton of six-membered aromatic rings being part of condensed ring systems formed by two rings
    • C07C309/35—Naphthalene sulfonic acids
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
    • C07B2200/00—Indexing scheme relating to specific properties of organic compounds
    • C07B2200/13—Crystalline forms, e.g. polymorphs

Definitions

  • the 5-year relative survival rate for cancer patients diagnosed in 1996-2003 is approximately two-thirds, up from about one half in 1975-1977 (Cancer Facts & Figures, American Cancer Society: Atlanta, Ga. (2008)).
  • the rate of new cancer cases decreased by an average 0.6% per year among men between 2000 and 2009, but stayed the same for women. From 2000 through 2009, death rates from all cancers combined decreased on average 1.8% per year among men and 1.4% per year among women.
  • This improvement in survival reflects progress in diagnosing at an earlier stage as well as improvements in treatment, for which there remains a need. Discovering highly effective anticancer agents with low toxicity is a primary goal of cancer research.
  • MEK Mitogen-activated protein kinase
  • salt forms e.g., crystalline salt forms
  • Compound 1 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen-2- one, hereinafter referred to as Compound 1.
  • pharmaceutical compositions comprising one or more salt forms of Compound 1 are also provided.
  • Compound 1 and uses thereof are disclosed in International Application Serial No.
  • FIGURE 1A depicts an X-ray powder diffraction pattern (XRPD) for potassium salt Form I of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one.
  • XRPD X-ray powder diffraction pattern
  • FIGURE 1B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for potassium salt Form I of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one.
  • FIGURE 1C depicts the NMR spectrum for potassium salt Form I of 3-[[3-fluoro- 2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one.
  • FIGURE 1D depicts the ultra performance liquid chromatography (hereinafter UPLC) results for potassium salt Form I of 3-[[3-fluoro-2-(methylsulfamoylamino)-4- pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one.
  • UPLC ultra performance liquid chromatography
  • FIGURE 1E depicts a variable temperature X-ray powder diffraction (hereinafter VT-XRPD) overlay pattern for potassium salt Form I of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one.
  • VT-XRPD variable temperature X-ray powder diffraction
  • FIGURE 2A depicts an X-ray powder diffraction pattern (XRPD) for potassium salt Form II of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one.
  • FIGURE 2B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for potassium salt Form II of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one.
  • DSC differential scanning calorimetry
  • TGA thermogravimetric analysis
  • FIGURE 2C depicts the NMR spectrum for potassium salt Form II of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one.
  • FIGURE 2D depicts the UPLC results for potassium salt Form II of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one.
  • FIGURE 2E depicts a VT-XRPD overlay pattern for potassium salt Form II of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one.
  • FIGURE 3A depicts an X-ray powder diffraction pattern (XRPD) for potassium salt Form III of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one.
  • XRPD X-ray powder diffraction pattern
  • FIGURE 3B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for potassium salt Form III of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one.
  • FIGURE 3C depicts the NMR spectrum for potassium salt Form III of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one.
  • FIGURE 3D depicts the UPLC results for potassium salt Form III of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 3 ME1 ⁇ 53438692.v1 136867-00920
  • FIGURE 3E depicts a VT-XRPD overlay pattern for potassium salt Form III of 3- [[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4- methyl-chromen-2-one.
  • FIGURE 3F depicts a XRPD overlay pattern for potassium salt Forms I, II and III of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4- methyl-chromen-2-one.
  • FIGURE 4A depicts an X-ray powder diffraction pattern (XRPD) for sodium salt Form II of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one.
  • XRPD X-ray powder diffraction pattern
  • FIGURE 4B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for sodium salt Form II of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one.
  • FIGURE 4C depicts the NMR spectrum for sodium salt Form II of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one.
  • FIGURE 4D depicts the UPLC results for sodium salt Form II of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one.
  • FIGURE 4E depicts a VT-XRPD overlay pattern for sodium salt Form II of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one.
  • FIGURE 4F depicts a XRPD overlay pattern for sodium salt Forms I and II of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one, before and after drying.
  • FIGURE 4G depicts a XRPD overlay pattern for sodium salt Forms I to VII of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one.
  • FIGURE 4H depicts an X-ray powder diffraction pattern (XRPD) for sodium salt Form I of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one.
  • XRPD X-ray powder diffraction pattern
  • FIGURE 5A depicts an X-ray powder diffraction pattern (XRPD) for sodium salt Form III of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one.
  • XRPD X-ray powder diffraction pattern
  • FIGURE 5B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for sodium salt Form III of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one.
  • FIGURE 5C depicts the NMR spectrum for sodium salt Form III of 3-[[3-fluoro- 2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one.
  • FIGURE 5D depicts the UPLC results for sodium salt Form III of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one.
  • FIGURE 6 depicts an X-ray powder diffraction pattern (XRPD) for sodium salt Form IV of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]- 4-methyl-chromen-2-one.
  • XRPD X-ray powder diffraction pattern
  • FIGURE 7A depicts an X-ray powder diffraction pattern (XRPD) for sodium salt Form V of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one.
  • FIGURE 7B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for sodium salt Form V of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one.
  • DSC differential scanning calorimetry
  • TGA thermogravimetric analysis
  • FIGURE 7C depicts the NMR spectrum for sodium salt Form V of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one.
  • FIGURE 7D depicts the UPLC results for sodium salt Form V of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one.
  • FIGURE 7E depicts a VT-XRPD overlay pattern for sodium salt Form V of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one.
  • FIGURE 8A depicts an X-ray powder diffraction pattern (XRPD) for sodium salt Form VI of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one.
  • FIGURE 8B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for sodium salt Form VI of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one.
  • FIGURE 8C depicts the NMR spectrum for sodium salt Form VI of 3-[[3-fluoro- 2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one.
  • FIGURE 8D depicts the UPLC results for sodium salt Form VI of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one.
  • FIGURE 9A depicts an X-ray powder diffraction pattern (XRPD) for sodium salt Form VII of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one.
  • XRPD X-ray powder diffraction pattern
  • FIGURE 9B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for sodium salt Form VII of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one.
  • FIGURE 9C depicts the NMR spectrum for sodium salt Form VII of 3-[[3-fluoro- 2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one.
  • FIGURE 9D depicts the UPLC results for sodium salt Form VII of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one.
  • FIGURE 9E depicts a VT-XRPD overlay pattern for sodium salt Form VII of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one.
  • FIGURE 10A depicts an X-ray powder diffraction pattern (XRPD) for calcium salt Form I of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one.
  • XRPD X-ray powder diffraction pattern
  • FIGURE 10B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for calcium salt Form I of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one.
  • FIGURE 10C depicts the NMR spectrum for calcium salt Form I of 3-[[3-fluoro- 2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one.
  • FIGURE 10D depicts the UPLC results for calcium salt Form I of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one.
  • FIGURE 10E depicts a VT-XRPD overlay pattern for calcium salt Form I of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one.
  • FIGURE 10F depicts a XRPD overlay pattern for calcium salt Forms I to V of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one.
  • FIGURE 11A depicts an X-ray powder diffraction pattern (XRPD) for calcium salt Form II of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one.
  • XRPD X-ray powder diffraction pattern
  • FIGURE 11B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for calcium salt Form II of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one.
  • FIGURE 11C depicts the NMR spectrum for calcium salt Form II of 3-[[3-fluoro- 2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one.
  • FIGURE 11D depicts the UPLC results for calcium salt Form II of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one.
  • FIGURE 11E depicts a VT-XRPD overlay pattern for calcium salt Form II of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one.
  • FIGURE 12A depicts an X-ray powder diffraction pattern (XRPD) for calcium salt Form III of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one.
  • XRPD X-ray powder diffraction pattern
  • FIGURE 12B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for calcium salt Form III of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one.
  • FIGURE 12C depicts the NMR spectrum for calcium salt Form III of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one.
  • FIGURE 12D depicts the UPLC results for calcium salt Form III of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one.
  • FIGURE 12E depicts a VT-XRPD overlay pattern for calcium salt Form III of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one.
  • FIGURE 13A depicts an X-ray powder diffraction pattern (XRPD) for calcium salt Form IV of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one.
  • FIGURE 13B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for calcium salt Form IV of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one.
  • DSC differential scanning calorimetry
  • TGA thermogravimetric analysis
  • FIGURE 13C depicts the NMR spectrum for calcium salt Form IV of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one.
  • FIGURE 13D depicts the UPLC results for calcium salt Form IV of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one.
  • FIGURE 13E depicts an XRPD overlay pattern for calcium salt Form IV of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one, before and after storage.
  • FIGURE 13F depicts a VT-XRPD overlay pattern for calcium salt Form V of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one.
  • FIGURE 14 depicts an X-ray powder diffraction pattern (XRPD) for calcium salt Form V of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one.
  • FIGURE 15A depicts an X-ray powder diffraction pattern (XRPD) for Choline salt Form I of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one.
  • FIGURE 15B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for Choline salt Form I of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one.
  • FIGURE 15C depicts the NMR spectrum for Choline salt Form I of 3-[[3-fluoro- 2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one.
  • FIGURE 15D depicts the UPLC results for Choline salt Form I of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one.
  • FIGURE 15E depicts a VT-XRPD overlay pattern for Choline salt Form I of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one.
  • FIGURE 15F depicts a XRPD overlay pattern for Choline salt Forms I - VI of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one.
  • FIGURE 16A depicts an X-ray powder diffraction pattern (XRPD) for Choline salt Form II of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one.
  • XRPD X-ray powder diffraction pattern
  • FIGURE 16B depicts an XRPD overlay pattern for Choline salt Form II of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one, before and after drying.
  • FIGURE 17A depicts an X-ray powder diffraction pattern (XRPD) for choline salt Form III of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one.
  • XRPD X-ray powder diffraction pattern
  • FIGURE 17D depicts the UPLC results for Choline salt Form III of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one.
  • FIGURE 17E depicts a VT-XRPD overlay pattern for Choline salt Form III of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one.
  • FIGURE 18A depicts an X-ray powder diffraction pattern (XRPD) for choline salt Form IV of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one.
  • FIGURE 18B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for choline salt Form IV of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one.
  • DSC differential scanning calorimetry
  • TGA thermogravimetric analysis
  • FIGURE 18C depicts the NMR spectrum for Choline salt Form IV of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one.
  • FIGURE 18D depicts the UPLC results for Choline salt Form IV of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one.
  • FIGURE 18E depicts a VT-XRPD overlay pattern for Choline salt Form IV of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one.
  • FIGURE 19A depicts an X-ray powder diffraction pattern (XRPD) for choline salt Form V of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one.
  • XRPD X-ray powder diffraction pattern
  • FIGURE 19B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for choline salt Form V of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one.
  • FIGURE 19C depicts the NMR spectrum for Choline salt Form V of 3-[[3-fluoro- 2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one.
  • FIGURE 19D depicts the UPLC results for Choline salt Form V of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one.
  • FIGURE 20A depicts an X-ray powder diffraction pattern (XRPD) for choline salt Form VI of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one.
  • XRPD X-ray powder diffraction pattern
  • FIGURE 20B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for choline salt Form VI of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one.
  • FIGURE 20C depicts the NMR spectrum for Choline salt Form VI of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one.
  • FIGURE 20D depicts the UPLC results for Choline salt Form VI of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one.
  • FIGURE 21A depicts an X-ray powder diffraction pattern (XRPD) for hydrogen bromide salt Form I of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3- fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one.
  • XRPD X-ray powder diffraction pattern
  • FIGURE 21B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for hydrogen bromide salt Form I of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one.
  • DSC differential scanning calorimetry
  • TGA thermogravimetric analysis
  • FIGURE 21C depicts the 1 H NMR spectrum for hydrogen bromide salt Form I of 3- [[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4- methyl-chromen-2-one.
  • FIGURE 21D depicts the UPLC results for hydrogen bromide salt Form I of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one.
  • FIGURE 21E depicts a XRPD overlay pattern for hydrogen bromide salt Forms I-III of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4- methyl-chromen-2-one.
  • FIGURE 22A depicts an X-ray powder diffraction pattern (XRPD) for hydrogen bromide salt Form II of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3- fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one.
  • XRPD X-ray powder diffraction pattern
  • FIGURE 22B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for hydrogen bromide salt Form II of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one.
  • FIGURE 22C depicts the NMR spectrum for hydrogen bromide salt Form II of 3- [[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4- methyl-chromen-2-one.
  • FIGURE 22D depicts the UPLC results for hydrogen bromide salt Form II of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one.
  • FIGURE 22E depicts a VT-XRPD overlay pattern for hydrogen bromide salt Form II of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4- methyl-chromen-2-one.
  • FIGURE 23A depicts an X-ray powder diffraction pattern (XRPD) for hydrogen bromide salt Form III of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3- fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one.
  • FIGURE 23B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for hydrogen bromide salt Form III of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one.
  • DSC differential scanning calorimetry
  • TGA thermogravimetric analysis
  • FIGURE 24A depicts an X-ray powder diffraction pattern (XRPD) for 1,5- naphthalenedisulfonate salt Form I of 3-[[3-fluoro-2-(methylsulfamoylamino)-4- pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one.
  • XRPD X-ray powder diffraction pattern
  • FIGURE 24B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for 1,5-naphthalenedisulfonate salt Form I of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one.
  • DSC differential scanning calorimetry
  • TGA thermogravimetric analysis
  • FIGURE 24C depicts the NMR spectrum for naphthalenedisulfonate salt Form I of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4- methyl-chromen-2-one.
  • FIGURE 24D depicts the UPLC results for naphthalenedisulfonate salt Form I of 3- [[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4- methyl-chromen-2-one.
  • FIGURE 25A depicts an X-ray powder diffraction pattern (XRPD) for 1,5- naphthalenedisulfonate salt Form II of 3-[[3-fluoro-2-(methylsulfamoylamino)-4- pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one.
  • XRPD X-ray powder diffraction pattern
  • FIGURE 25B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for 1,5-naphthalenedisulfonate salt Form II of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one.
  • DSC differential scanning calorimetry
  • TGA thermogravimetric analysis
  • FIGURE 25C depicts the NMR spectrum for naphthalenedisulfonate salt Form II of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4- methyl-chromen-2-one.
  • FIGURE 25D depicts the UPLC results for naphthalenedisulfonate salt Form II of 3- [[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4- methyl-chromen-2-one.
  • FIGURE 26A depicts an X-ray powder diffraction pattern (XRPD) for edisylate salt Form I of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one.
  • XRPD X-ray powder diffraction pattern
  • FIGURE 26B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for edisylate salt Form I of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one.
  • DSC differential scanning calorimetry
  • TGA thermogravimetric analysis
  • FIGURE 26C depicts the 1 H NMR spectrum for edisylate salt Form I of 3-[[3-fluoro- 2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one.
  • FIGURE 26D depicts the UPLC results for edisylate salt Form I of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one.
  • FIGURE 27A depicts an X-ray powder diffraction pattern (XRPD) for edisylate salt Form II of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one.
  • XRPD X-ray powder diffraction pattern
  • FIGURE 27B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for edisylate salt Form II of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one.
  • FIGURE 27C depicts the NMR spectrum for edisylate salt Form II of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one.
  • FIGURE 27D depicts the UPLC results for edisylate salt Form II of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one.
  • FIGURE 28A depicts an X-ray powder diffraction pattern (XRPD) for diethylamine salt Form I of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one.
  • XRPD X-ray powder diffraction pattern
  • FIGURE 28B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for diethylamine salt Form I of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one.
  • FIGURE 28C depicts the NMR spectrum for diethylamine salt Form I of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one.
  • FIGURE 28D depicts the UPLC results for diethylamine salt Form I of 3-[[3-fluoro- 2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one.
  • FIGURE 28E depicts a VT-XRPD overlay pattern for diethylamine salt Form I of 3- [[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4- methyl-chromen-2-one.
  • FIGURE 29A depicts an X-ray powder diffraction pattern (XRPD) for diethylamine salt Form II of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one.
  • XRPD X-ray powder diffraction pattern
  • FIGURE 29B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for diethylamine salt Form II of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one.
  • FIGURE 29C depicts the NMR spectrum for diethylamine salt Form II of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one.
  • FIGURE 29D depicts the UPLC results for diethylamine salt Form II of 3-[[3-fluoro- 2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one.
  • FIGURE 29E depicts a VT-XRPD overlay pattern for diethylamine salt Form II of 3- [[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4- methyl-chromen-2-one.
  • FIGURE 30A depicts an X-ray powder diffraction pattern (XRPD) for hydrogen chloride salt Form I of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3- fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one.
  • FIGURE 30B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for hydrogen chloride salt Form I of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one.
  • DSC differential scanning calorimetry
  • TGA thermogravimetric analysis
  • FIGURE 30C depicts the NMR spectrum for hydrogen chloride salt Form I of 3- [[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4- methyl-chromen-2-one.
  • FIGURE 30D depicts the UPLC results for hydrogen chloride salt Form I of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one.
  • FIGURE 31 depicts an X-ray powder diffraction pattern (XRPD) for hydrogen chloride salt Form II of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3- fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one.
  • XRPD X-ray powder diffraction pattern
  • FIGURE 32 depicts an X-ray powder diffraction pattern (XRPD) for hydrogen chloride salt Form III of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3- fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one.
  • FIGURE 33A depicts an X-ray powder diffraction pattern (XRPD) for hydrogen chloride salt Form IV of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3- fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one.
  • FIGURE 33B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for hydrogen chloride salt Form IV of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one.
  • FIGURE 33C depicts the NMR spectrum for hydrogen chloride salt Form IV of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4- methyl-chromen-2-one.
  • FIGURE 33D depicts the UPLC results for hydrogen chloride salt Form IV of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one.
  • FIGURE 33E depicts a XRPD overlay pattern for hydrogen chloride salt Form IV of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4- methyl-chromen-2-one, before and after drying.
  • FIGURE 34A depicts X-ray powder diffraction (XRPD) patterns for reference sample free Form I of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3- fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one, and for the solid starting material used in salt screening described in the present disclosure.
  • FIGURE 34B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for reference sample free Form I , the solid starting material used in salt screening described in the present disclosure.
  • DSC differential scanning calorimetry
  • TGA thermogravimetric analysis
  • FIGURE 35A depicts X-ray powder diffraction (XRPD) overlay patterns for reference sample potassium salt Form I of 3-[[3-fluoro-2-(methylsulfamoylamino)-4- pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one, and for the re- prepared sample of potassium salt Form I.
  • XRPD X-ray powder diffraction
  • FIGURE 35B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for the re-prepared sample of potassium salt Form I of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one.
  • DSC differential scanning calorimetry
  • TGA thermogravimetric analysis
  • FIGURE 36A depicts X-ray powder diffraction (XRPD) overlay patterns for reference sample sodium salt Form II of 3-[[3-fluoro-2-(methylsulfamoylamino)-4- pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one, and for the re- prepared sample of sodium salt Form II.
  • XRPD X-ray powder diffraction
  • FIGURE 36B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for the re-prepared sample of sodium salt Form II of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one.
  • DSC differential scanning calorimetry
  • TGA thermogravimetric analysis
  • FIGURE 37A depicts X-ray powder diffraction (XRPD) overlay patterns for reference sample calcium salt Form II of 3-[[3-fluoro-2-(methylsulfamoylamino)-4- pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one, and for the re- prepared sample of calcium salt Form II.
  • XRPD X-ray powder diffraction
  • FIGURE 37B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for the re-prepared sample of calcium salt Form II of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one.
  • DSC differential scanning calorimetry
  • TGA thermogravimetric analysis
  • FIGURE 38A depicts X-ray powder diffraction (XRPD) overlay patterns for reference sample choline salt Form I of 3-[[3-fluoro-2-(methylsulfamoylamino)-4- pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one, and for the re- prepared sample of choline salt Form I.
  • XRPD X-ray powder diffraction
  • FIGURE 38B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for the re-prepared sample of choline salt Form I of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one.
  • DSC differential scanning calorimetry
  • TGA thermogravimetric analysis
  • FIGURE 39A depicts X-ray powder diffraction (XRPD) overlay patterns for reference sample hydrogen bromide salt Form II of 3-[[3-fluoro-2-(methylsulfamoylamino)- 4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one, and for the re- prepared sample of hydrogen bromide salt Form II.
  • XRPD X-ray powder diffraction
  • FIGURE 39B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for the re-prepared sample of hydrogen bromide salt Form II of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4- methyl-chromen-2-one.
  • FIGURE 40 depicts structures of selected the counter-ions/co-formers used in the salt screening experiments. DETAILED DESCRIPTION Provided are salt forms of Compound 1.
  • “Compound 1” and 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one are used interchangeably, and each refer to the compound having the following chemical structure: .
  • “crystalline” refers to a solid form of a compound wherein there exists long-range atomic order in the positions of the atoms. The crystalline nature of a solid can be confirmed, for example, by examination of the X-ray powder diffraction pattern.
  • a salt can be a solvate or anhydrate.
  • Solid refers to a salt form which incorporates solvent within the three dimensional configuration; commonly a stoichiometric amount of solvent relative to Compound 1 is incorporated within the three dimensional configuration.
  • Hydrophilic refers to a solvate wherein the solvent is water.
  • Hydrate refers to a salt form that is characterized by the substantial absence water, e.g., less than 1% by weight as determined by Karl Fisher analysis, within the crystal structure. “Substantial absence of solvent” within the crystal structure includes less than 0.25 molar equivalents, and less than 0.1 molar equivalents of solvent relative to Compound 1.
  • the salts of Compound 1 described herein are selected from potassium salts, sodium salts, calcium salts, choline salts, hydrogen bromide salts, 1,5- naphthalenedisulfonate salts, edisylate salts, diethylamine salts, and hydrogen chloride salts.
  • the salts of Compound 1 described herein are selected from potassium salt Forms I, II, and III; sodium salt Forms II, III, IV, V, VI, and VII; calcium salt Forms I, II, III, IV, and V; choline salt Forms I, II, III, IV, V, and VI; hydrogen bromide salt 18 ME1 ⁇ 53438692.v1 136867-00920 Forms I, II, and III; 1,5-naphthalenedisulfonate salt Forms I and II; edisylate salt Forms I and II, diethylamine salt Forms I and II; and hydrogen chloride salt Forms I, II, III, and IV.
  • the salts of Compound 1 described herein are crystalline.
  • the salts of Compound 1 are each a single crystalline form.
  • a “single crystalline form” means that the recited compound, i.e., Compound 1, is present as a single crystal or a plurality of crystals in which each crystal has the same crystal form (e.g., Form I or Form II). Percent by weight of a particular crystal form is determined by the weight of the particular crystal form divided by the sum weight of the particular crystal, plus the weight of the other crystal form(s) present plus the weight of amorphous form, if present, multiplied by 100%. In some instances, each crystalline form as described herein is at least 60%, at least 70%, at least 80%, at least 90%, at least 95%, or at least 99% a single crystalline form.
  • “Pure single crystalline form” means that Compound 1 is present as a single crystal or a plurality of crystals in which each crystal has the same crystal form with no other detectable amounts of other crystal forms present and/or amorphous forms.
  • the term “amorphous” refers to a solid that is present in a non-crystalline state or form. Amorphous solids are disordered arrangements of molecules and therefore possess no distinguishable crystal lattice or unit cell and consequently have no definable long range ordering. Solid state ordering of solids may be determined by standard techniques known in the art, e.g., by X-ray powder diffraction (XRPD) or differential scanning calorimetry (DSC).
  • the 2-theta (2 ⁇ ) values of the X-ray powder diffraction patterns for the crystalline forms described herein may vary slightly from one instrument to another and also depending on variations in sample preparation and batch to batch variation due to factors such as temperature variation, sample displacement, and the presence or absence of an internal standard. Therefore, unless otherwise defined, the XRPD patterns / assignments recited herein are not to be construed as absolute and can vary ⁇ 0.2 degrees. It is well known in the art that this variability will account for the above factors without hindering the unequivocal identification of a crystal form. Unless otherwise specified, the 2-theta values provided herein were obtained using Cu K ⁇ 1 radiation.
  • Substantially the same XRPD pattern” or “an X-ray powder diffraction pattern substantially similar to” a defined figure means that for comparison purposes, at least 90% of the peaks shown are present. It is to be further understood that for comparison purposes some variability in peak intensities from those shown are allowed, such as ⁇ 5% of the intensity of the most intense peak. 19 ME1 ⁇ 53438692.v1 136867-00920 Temperature values, e.g., for DSC peaks herein may vary slightly from one instrument to another and also depending on variations in sample preparation, batch to batch variation, and environmental factors. Therefore, unless otherwise defined, temperature values recited herein are not to be construed as absolute and can vary ⁇ 5 degrees or ⁇ 2 degrees Celsius.
  • potassium salt crystalline Form I is characterized by at least three x-ray powder diffraction peaks at 2 ⁇ angles selected from 4.5°, 8.9°, 14.6°, 17.2°, 17.8°, 23.5°, and 23.8°. In another embodiment, potassium salt crystalline Form I is characterized by at least four x-ray powder diffraction peaks at 2 ⁇ angles selected from 4.5°, 8.9°, 14.6°, 17.2°, 17.8°, 23.5°, and 23.8°.
  • potassium salt crystalline Form I is characterized by at least five x-ray powder diffraction peaks at 2 ⁇ angles selected from 4.5°, 8.9°, 14.6°, 17.2°, 17.8°, 23.5°, and 23.8°. In another embodiment, potassium salt crystalline Form I is characterized by at least six x-ray powder diffraction peaks at 2 ⁇ angles selected from 4.5°, 8.9°, 14.6°, 17.2°, 17.8°, 23.5°, and 23.8°. In another embodiment, potassium salt crystalline Form I is characterized by x-ray powder diffraction peaks at 2 ⁇ angles 4.5°, 8.9°, 14.6°, 17.2°, 17.8°, 23.5°, and 23.8°.
  • potassium salt crystalline Form I is characterized by at least three, four, five, six, or all x-ray powder diffraction peaks at 2 ⁇ angles selected from 4.5°, 8.9°, 14.6°, 17.2°, 17.8°, 23.5°, and 23.8°, and is further characterized by one or more x-ray powder diffraction peaks at 2 ⁇ angles selected from 7.3°, 10.6°, 19.3°, 22.1°, and 22.4°.
  • potassium salt crystalline Form I is characterized by one or more, or all of the x-ray powder diffraction peaks at 2 ⁇ angles provided in Table 11A.
  • potassium salt crystalline Form I is characterized by an x-ray powder diffraction substantially similar to Figure 1A.
  • potassium salt crystalline Form I is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 1A, or the peaks recited in Table 11A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising a peak endotherm at 246.1 °C ⁇ 2 °C.
  • the molar ratio of potassium counter-ion to compound in potassium salt crystalline Form I is about 0.9
  • potassium salt crystalline Form I is further characterized by the features in any one of the previous two paragraphs, Figure 1A, or the peaks recited in Table 11A.
  • potassium salt crystalline Form I is an anhydrate, and is further characterized by the features in any one of the previous three paragraphs, Figure 1A, or the peaks recited in Table 11A.
  • Potassium Salt Form II In one embodiment, potassium salt crystalline Form II is characterized by at least three x-ray powder diffraction peaks at 2 ⁇ angles selected from 4.4°, 8.6°, 14.4°, 17.5°, 18.4°, 21.5°, and 24.0°.
  • potassium salt crystalline Form II is characterized by at least four x-ray powder diffraction peaks at 2 ⁇ angles selected from 4.4°, 8.6°, 14.4°, 17.5°, 18.4°, 21.5°, and 24.0°. In another embodiment, potassium salt crystalline Form II is characterized by at least five x-ray powder diffraction peaks at 2 ⁇ angles selected from 4.4°, 8.6°, 14.4°, 17.5°, 18.4°, 21.5°, and 24.0°. In another embodiment, potassium salt crystalline Form II is characterized by at least six x-ray powder diffraction peaks at 2 ⁇ angles selected from 4.4°, 8.6°, 14.4°, 17.5°, 18.4°, 21.5°, and 24.0°.
  • potassium salt crystalline Form II is characterized by x-ray powder diffraction peaks at 2 ⁇ angles 4.4°, 8.6°, 14.4°, 17.5°, 18.4°, 21.5°, and 24.0°.
  • potassium salt crystalline Form II is characterized by at least three, four, five, six, or all x-ray powder diffraction peaks at 2 ⁇ angles selected from 4.4°, 8.6°, 14.4°, 17.5°, 18.4°, 21.5°, and 24.0°, and is further characterized by one or more x-ray powder diffraction peaks at 2 ⁇ angles selected from 7.8°, 17.2°, 18.9°, 23.5°, and 27.6°.
  • potassium salt crystalline Form II is characterized by one or more, or all of the x-ray powder diffraction peaks at 2 ⁇ angles provided in Table 12A. In another embodiment, potassium salt crystalline Form II is characterized by an x-ray powder diffraction substantially similar to Figure 2A. In another embodiment, potassium salt crystalline Form II is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 2A, or the peaks recited in Table 12A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising a peak endotherm at 257.9 °C ⁇ 2 °C.
  • DSC differential scanning calorimeter
  • the molar ratio of potassium counter-ion to compound in potassium salt crystalline Form II is about 1, and potassium salt crystalline Form II is further characterized by the features in any one of the previous two paragraphs, Figure 2A, or the peaks recited in Table 12A.
  • potassium salt crystalline Form II is an anhydrate, and is further characterized by the features in any one of the previous three paragraphs, Figure 2A, or the peaks recited in Table 12A.
  • potassium salt crystalline Form III is characterized by at least three x-ray powder diffraction peaks at 2 ⁇ angles selected from 7.2°, 9.3°, 10.2°, 13.6°, 15.0°, 17.0°, and 20.4°. In another embodiment, potassium salt crystalline Form III is characterized by at least four x-ray powder diffraction peaks at 2 ⁇ angles selected from 7.2°, 9.3°, 10.2°, 13.6°, 15.0°, 17.0°, and 20.4°.
  • potassium salt crystalline Form III is characterized by at least five x-ray powder diffraction peaks at 2 ⁇ angles selected from 7.2°, 9.3°, 10.2°, 13.6°, 15.0°, 17.0°, and 20.4°. In another embodiment, potassium salt crystalline Form III is characterized by at least six x-ray powder diffraction peaks at 2 ⁇ angles selected from 7.2°, 9.3°, 10.2°, 13.6°, 15.0°, 17.0°, and 20.4°. In another embodiment, potassium salt crystalline Form III is characterized by x-ray powder diffraction peaks at 2 ⁇ angles 7.2°, 9.3°, 10.2°, 13.6°, 15.0°, 17.0°, and 20.4°.
  • potassium salt crystalline Form III is characterized by at least three, four, five, six, or all x-ray powder diffraction peaks at 2 ⁇ angles selected from 7.2°, 9.3°, 10.2°, 13.6°, 15.0°, 17.0°, and 20.4°, and is further characterized by one or more x-ray powder diffraction peaks at 2 ⁇ angles selected from 12.0°, 13.2°, 17.7°, and 23.9°.
  • potassium salt crystalline Form III is characterized by one or more, or all of the x-ray powder diffraction peaks at 2 ⁇ angles provided in Table 13A.
  • potassium salt crystalline Form III is characterized by an x-ray powder diffraction substantially similar to Figure 3A.
  • potassium salt crystalline Form III is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 3A, or the peaks recited in Table 13A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 149.0 °C, 161.3 °C, and 267.5 °C ⁇ 2 °C.
  • the molar ratio of potassium counter-ion to compound in potassium salt crystalline Form III is about 0.9
  • potassium salt crystalline Form III is further characterized by the features in any one of the previous two paragraphs, Figure 3A, or the peaks recited in Table 13A.
  • potassium salt crystalline Form III is a DMSO solvate, and is further characterized by the features in any one of the previous three paragraphs, Figure 3A, or the peaks recited in Table 13A.
  • Sodium Salt Form II In one embodiment, sodium salt crystalline Form II is characterized by at least three x-ray powder diffraction peaks at 2 ⁇ angles selected from 6.5°, 7.6°, 14.7°, 15.2°, and 22.9°. 22 ME1 ⁇ 53438692.v1 136867-00920 In another embodiment, sodium salt crystalline Form II is characterized by at least four x-ray powder diffraction peaks at 2 ⁇ angles selected from 6.5°, 7.6°, 14.7°, 15.2°, and 22.9°.
  • sodium salt crystalline Form II is characterized by x-ray powder diffraction peaks at 2 ⁇ angles 6.5°, 7.6°, 14.7°, 15.2°, and 22.9°.
  • sodium salt crystalline Form II is characterized by at least three, four, or all x-ray powder diffraction peaks at 2 ⁇ angles selected from 6.5°, 7.6°, 14.7°, 15.2°, and 22.9°, and is further characterized by one or more x-ray powder diffraction peaks at 2 ⁇ angles selected from 8.4°, 17.1°, and 18.0°.
  • sodium salt crystalline Form II is characterized by one or more, or all of the x-ray powder diffraction peaks at 2 ⁇ angles provided in Table 15A.
  • sodium salt crystalline Form II is characterized by an x-ray powder diffraction substantially similar to Figure 4A.
  • sodium salt crystalline Form II is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 4A, or the peaks recited in Table 15A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 65.3 °C, 118.5 °C, and 179.3 °C ⁇ 2 °C.
  • DSC differential scanning calorimeter
  • the molar ratio of sodium counter-ion to compound in sodium salt crystalline Form II is about 1.1, and sodium salt crystalline Form II is further characterized by the features in any one of the previous two paragraphs, Figure 4A, or the peaks recited in Table 15A.
  • sodium salt crystalline Form II is a hydrate, and is further characterized by the features in any one of the previous three paragraphs, Figure 4A, or the peaks recited in Table 15A.
  • Sodium Salt Form III In one embodiment, sodium salt crystalline Form III is characterized by at least three x-ray powder diffraction peaks at 2 ⁇ angles selected from 9.7°, 9.9°, 15.3°, 17.8°, 18.6°, 19.0°, 22.9°, and 23.6°.
  • sodium salt crystalline Form III is characterized by at least four x-ray powder diffraction peaks at 2 ⁇ angles selected from 9.7°, 9.9°, 15.3°, 17.8°, 18.6°, 19.0°, 22.9°, and 23.6°.
  • sodium salt crystalline Form III is characterized by at least five x-ray powder diffraction peaks at 2 ⁇ angles selected from 9.7°, 9.9°, 15.3°, 17.8°, 18.6°, 19.0°, 22.9°, and 23.6°.
  • sodium salt crystalline Form III is characterized by at least six x-ray powder diffraction peaks at 2 ⁇ angles selected from 9.7°, 9.9°, 15.3°, 17.8°, 18.6°, 19.0°, 22.9°, and 23.6°.
  • sodium salt crystalline Form III is characterized by at least 23 ME1 ⁇ 53438692.v1 136867-00920 seven x-ray powder diffraction peaks at 2 ⁇ angles selected from 9.7°, 9.9°, 15.3°, 17.8°, 18.6°, 19.0°, 22.9°, and 23.6°.
  • sodium salt crystalline Form III is characterized by x-ray powder diffraction peaks at 2 ⁇ angles 9.7°, 9.9°, 15.3°, 17.8°, 18.6°, 19.0°, 22.9°, and 23.6°.
  • sodium salt crystalline Form III is characterized by at least three, four, five, six, seven, or all x-ray powder diffraction peaks at 2 ⁇ angles selected from 9.7°, 9.9°, 15.3°, 17.8°, 18.6°, 19.0°, 22.9°, and 23.6°, and is further characterized by one or more x-ray powder diffraction peaks at 2 ⁇ angles selected from 13.2°, 15.6°, 16.4°, 16.6°, 21.0°, 22.0°, and 22.5°.
  • sodium salt crystalline Form III is characterized by one or more, or all of the x-ray powder diffraction peaks at 2 ⁇ angles provided in Table 16A. In another embodiment, sodium salt crystalline Form III is characterized by an x-ray powder diffraction substantially similar to Figure 5A. In another embodiment, sodium salt crystalline Form III is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 5A, or the peaks recited in Table 16A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising a peak endotherm at 179.8 °C ⁇ 2 °C.
  • DSC differential scanning calorimeter
  • the molar ratio of sodium counter-ion to compound in sodium salt crystalline Form III is about 1.1, and sodium salt crystalline Form III is further characterized by the features in any one of the previous two paragraphs, Figure 5A, or the peaks recited in Table 16A.
  • sodium salt crystalline Form III is a DMSO solvate, and is further characterized by the features in any one of the previous three paragraphs, Figure 5A, or the peaks recited in Table 16A.
  • Sodium Salt Form IV In one embodiment, sodium salt crystalline Form IV is characterized by at least three x-ray powder diffraction peaks at 2 ⁇ angles selected from 8.0°, 12.3°, 14.5°, 14.9°, 15.2°, 16.0°, and 24.7°.
  • sodium salt crystalline Form IV is characterized by at least four x-ray powder diffraction peaks at 2 ⁇ angles selected from 8.0°, 12.3°, 14.5°, 14.9°, 15.2°, 16.0°, and 24.7°. In another embodiment, sodium salt crystalline Form IV is characterized by at least five x-ray powder diffraction peaks at 2 ⁇ angles selected from 8.0°, 12.3°, 14.5°, 14.9°, 15.2°, 16.0°, and 24.7°. In another embodiment, sodium salt crystalline Form IV is characterized by at least six x-ray powder diffraction peaks at 2 ⁇ angles selected from 8.0°, 12.3°, 14.5°, 14.9°, 15.2°, 16.0°, and 24.7°.
  • sodium salt crystalline Form IV is characterized by x-ray powder diffraction peaks at 2 ⁇ angles 8.0°, 24 ME1 ⁇ 53438692.v1 136867-00920 12.3°, 14.5°, 14.9°, 15.2°, 16.0°, and 24.7°.
  • sodium salt crystalline Form IV is characterized by at least three, four, five, six, or all x-ray powder diffraction peaks at 2 ⁇ angles selected from 8.0°, 12.3°, 14.5°, 14.9°, 15.2°, 16.0°, and 24.7°, and is further characterized by one or more x-ray powder diffraction peaks at 2 ⁇ angles selected from 13.3°, 17.7°, 22.1°, 23.0°, and 29.4°.
  • sodium salt crystalline Form IV is characterized by one or more, or all of the x-ray powder diffraction peaks at 2 ⁇ angles provided in Table 17.
  • sodium salt crystalline Form IV is characterized by an x-ray powder diffraction substantially similar to Figure 6.
  • sodium salt crystalline Form V is characterized by at least three x-ray powder diffraction peaks at 2 ⁇ angles selected from 9.6°, 10.8°, 16.2°, 17.5°, 19.7°, 22.1°, 23.3°, and 24.3°.
  • sodium salt crystalline Form V is characterized by at least four x-ray powder diffraction peaks at 2 ⁇ angles selected from 9.6°, 10.8°, 16.2°, 17.5°, 19.7°, 22.1°, 23.3°, and 24.3°.
  • sodium salt crystalline Form V is characterized by at least five x-ray powder diffraction peaks at 2 ⁇ angles selected from 9.6°, 10.8°, 16.2°, 17.5°, 19.7°, 22.1°, 23.3°, and 24.3°.
  • sodium salt crystalline Form V is characterized by at least six x-ray powder diffraction peaks at 2 ⁇ angles selected from 9.6°, 10.8°, 16.2°, 17.5°, 19.7°, 22.1°, 23.3°, and 24.3°.
  • sodium salt crystalline Form V is characterized by at least seven x-ray powder diffraction peaks at 2 ⁇ angles selected from 9.6°, 10.8°, 16.2°, 17.5°, 19.7°, 22.1°, 23.3°, and 24.3°.
  • sodium salt crystalline Form V is characterized by x-ray powder diffraction peaks at 2 ⁇ angles 9.6°, 10.8°, 16.2°, 17.5°, 19.7°, 22.1°, 23.3°, and 24.3°.
  • sodium salt crystalline Form V is characterized by at least three, four, five, six, seven, or all x-ray powder diffraction peaks at 2 ⁇ angles selected from 9.6°, 10.8°, 16.2°, 17.5°, 19.7°, 22.1°, 23.3°, and 24.3°, and is further characterized by one or more x-ray powder diffraction peaks at 2 ⁇ angles selected from 14.6°, 16.9°, 17.2°, 17.9°, 18.4°, 19.0°, 23.5°, and 29.5°.
  • sodium salt crystalline Form V is characterized by one or more, or all of the x-ray powder diffraction peaks at 2 ⁇ angles provided in Table 18A.
  • sodium salt crystalline Form V is characterized by an x-ray powder diffraction substantially similar to Figure 7A.
  • sodium salt crystalline Form V is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 7A, or the peaks recited in Table 25 ME1 ⁇ 53438692.v1 136867-00920 18A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 112.0 °C and 134.8 °C ⁇ 2 °C.
  • DSC differential scanning calorimeter
  • the molar ratio of sodium counter-ion to compound in sodium salt crystalline Form V is about 1.0, and sodium salt crystalline Form V is further characterized by the features in any one of the previous two paragraphs, Figure 7A, or the peaks recited in Table 18A.
  • sodium salt crystalline Form V is a H 2 O-NMP co-solvate, and is further characterized by the features in any one of the previous three paragraphs, Figure 7A, or the peaks recited in Table 18A.
  • sodium salt crystalline Form VI is characterized by at least three x-ray powder diffraction peaks at 2 ⁇ angles selected from 8.5°, 10.6°, 14.4°, 16.2°, 19.3°, 19.6°, 22.9°, and 23.3°.
  • sodium salt crystalline Form VI is characterized by at least four x-ray powder diffraction peaks at 2 ⁇ angles selected from 8.5°, 10.6°, 14.4°, 16.2°, 19.3°, 19.6°, 22.9°, and 23.3°.
  • sodium salt crystalline Form VI is characterized by at least five x-ray powder diffraction peaks at 2 ⁇ angles selected from 8.5°, 10.6°, 14.4°, 16.2°, 19.3°, 19.6°, 22.9°, and 23.3°.
  • sodium salt crystalline Form VI is characterized by at least six x-ray powder diffraction peaks at 2 ⁇ angles selected from 8.5°, 10.6°, 14.4°, 16.2°, 19.3°, 19.6°, 22.9°, and 23.3°.
  • sodium salt crystalline Form VI is characterized by at least seven x-ray powder diffraction peaks at 2 ⁇ angles selected from 8.5°, 10.6°, 14.4°, 16.2°, 19.3°, 19.6°, 22.9°, and 23.3°.
  • sodium salt crystalline Form VI is characterized by x-ray powder diffraction peaks at 2 ⁇ angles 8.5°, 10.6°, 14.4°, 16.2°, 19.3°, 19.6°, 22.9°, and 23.3°.
  • sodium salt crystalline Form VI is characterized by at least three, four, five, six, seven, or all x-ray powder diffraction peaks at 2 ⁇ angles selected from 8.5°, 10.6°, 14.4°, 16.2°, 19.3°, 19.6°, 22.9°, and 23.3°, and is further characterized by one or more x-ray powder diffraction peaks at 2 ⁇ angles selected from 6.4°, 6.7°, 9.7°, 12.9°, 15.2°, 17.2°, 18.3°, 20.4°, 21.4°, and 29.0°.
  • sodium salt crystalline Form VI is characterized by one or more, or all of the x-ray powder diffraction peaks at 2 ⁇ angles provided in Table 19A.
  • sodium salt crystalline Form VI is characterized by an x-ray powder diffraction substantially similar to Figure 8A.
  • sodium salt crystalline Form VI is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 8A, or the peaks recited in Table 26 ME1 ⁇ 53438692.v1 136867-00920 19A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 49.9 °C, 100.2 °C, 116.9 °C, and 154.6 °C ⁇ 2 °C.
  • DSC differential scanning calorimeter
  • the molar ratio of sodium counter-ion to compound in sodium salt crystalline Form VI is about 1.0, and sodium salt crystalline Form VI is further characterized by the features in any one of the previous two paragraphs, Figure 8A, or the peaks recited in Table 19A.
  • sodium salt crystalline Form VI is a DMAc solvate, and is further characterized by the features in any one of the previous three paragraphs, Figure 8A, or the peaks recited in Table 19A.
  • sodium salt crystalline Form VII is characterized by at least three x-ray powder diffraction peaks at 2 ⁇ angles selected from 9.6°, 9.9°, 15.5°, 17.2°, 18.1°, 22.3°, 23.2°, and 29.0°.
  • sodium salt crystalline Form VII is characterized by at least four x-ray powder diffraction peaks at 2 ⁇ angles selected from 9.6°, 9.9°, 15.5°, 17.2°, 18.1°, 22.3°, 23.2°, and 29.0°.
  • sodium salt crystalline Form VII is characterized by at least five x-ray powder diffraction peaks at 2 ⁇ angles selected from 9.6°, 9.9°, 15.5°, 17.2°, 18.1°, 22.3°, 23.2°, and 29.0°.
  • sodium salt crystalline Form VII is characterized by at least six x-ray powder diffraction peaks at 2 ⁇ angles selected from 9.6°, 9.9°, 15.5°, 17.2°, 18.1°, 22.3°, 23.2°, and 29.0°.
  • sodium salt crystalline Form VII is characterized by at least seven x-ray powder diffraction peaks at 2 ⁇ angles selected from 9.6°, 9.9°, 15.5°, 17.2°, 18.1°, 22.3°, 23.2°, and 29.0°.
  • sodium salt crystalline Form VII is characterized by x-ray powder diffraction peaks at 2 ⁇ angles 9.6°, 9.9°, 15.5°, 17.2°, 18.1°, 22.3°, 23.2°, and 29.0°.
  • sodium salt crystalline Form VII is characterized by at least three, four, five, six, seven, or all x-ray powder diffraction peaks at 2 ⁇ angles selected from 9.6°, 9.9°, 15.5°, 17.2°, 18.1°, 22.3°, 23.2°, and 29.0°, and is further characterized by one or more x-ray powder diffraction peaks at 2 ⁇ angles selected from 12.9°, 19.2°, 19.8°, 21.5°, 31.1°, and 32.0°.
  • sodium salt crystalline Form VII is characterized by one or more, or all of the x-ray powder diffraction peaks at 2 ⁇ angles provided in Table 20A.
  • sodium salt crystalline Form VII is characterized by an x-ray powder diffraction substantially similar to Figure 9A.
  • sodium salt crystalline Form VII is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 9A, or the peaks recited in Table 27 ME1 ⁇ 53438692.v1 136867-00920 20A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 154.7 °C, and 184.2 °C ⁇ 2 °C.
  • DSC differential scanning calorimeter
  • the molar ratio of sodium counter-ion to compound in sodium salt crystalline Form VII is about 1.0, and sodium salt crystalline Form VII is further characterized by the features in any one of the previous two paragraphs, Figure 9A, or the peaks recited in Table 20A.
  • sodium salt crystalline Form VII is an acetone solvate, and is further characterized by the features in any one of the previous three paragraphs, Figure 9A, or the peaks recited in Table 20A.
  • Calcium Salt Form I In one embodiment, calcium salt crystalline Form I is characterized by at least three x-ray powder diffraction peaks at 2 ⁇ angles selected from 6.4°, 7.0°, 12.5°, 14.0°, 17.3°, 18.0°, and 23.3°.
  • calcium salt crystalline Form I is characterized by at least four x-ray powder diffraction peaks at 2 ⁇ angles selected from 6.4°, 7.0°, 12.5°, 14.0°, 17.3°, 18.0°, and 23.3°. In another embodiment, calcium salt crystalline Form I is characterized by at least five x-ray powder diffraction peaks at 2 ⁇ angles selected from 6.4°, 7.0°, 12.5°, 14.0°, 17.3°, 18.0°, and 23.3°. In another embodiment, calcium salt crystalline Form I is characterized by at least six x-ray powder diffraction peaks at 2 ⁇ angles selected from 6.4°, 7.0°, 12.5°, 14.0°, 17.3°, 18.0°, and 23.3°.
  • calcium salt crystalline Form I is characterized by x-ray powder diffraction peaks at 2 ⁇ angles 6.4°, 7.0°, 12.5°, 14.0°, 17.3°, 18.0°, and 23.3°.
  • calcium salt crystalline Form I is characterized by at least three, four, five, six, or all x-ray powder diffraction peaks at 2 ⁇ angles selected from 6.4°, 7.0°, 12.5°, 14.0°, 17.3°, 18.0°, and 23.3°, and is further characterized by one or more x-ray powder diffraction peaks at 2 ⁇ angles selected from 4.3°, 7.7°, 8.2°, 9.3°, 12.8°, 15.8°, 18.8°, 20.1°, and 21.1°.
  • calcium salt crystalline Form I is characterized by one or more, or all of the x-ray powder diffraction peaks at 2 ⁇ angles provided in Table 22A. In another embodiment, calcium salt crystalline Form I is characterized by an x-ray powder diffraction substantially similar to Figure 10A. In another embodiment, calcium salt crystalline Form I is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 10A, or the peaks recited in Table 22A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 73.1 °C, 135.8 °C and 200.2 °C ⁇ 2 °C.
  • DSC differential scanning calorimeter
  • the molar ratio of calcium counter-ion to compound in calcium salt crystalline Form I is about 0.4, and calcium salt crystalline Form I is further characterized by the features in any one of the previous two paragraphs, Figure 10A, or the peaks recited in Table 22A.
  • calcium salt crystalline Form I is a hydrate, and is further characterized by the features in any one of the previous three paragraphs, Figure 10A, or the peaks recited in Table 22A.
  • calcium salt crystalline Form II is characterized by at least three x-ray powder diffraction peaks at 2 ⁇ angles selected from 4.3°, 8.3°, 8.6°, 13.0°, 14.0°, 15.9°, and 17.3°. In another embodiment, calcium salt crystalline Form II is characterized by at least four x-ray powder diffraction peaks at 2 ⁇ angles selected from 4.3°, 8.3°, 8.6°, 13.0°, 14.0°, 15.9°, and 17.3°.
  • calcium salt crystalline Form II is characterized by at least five x-ray powder diffraction peaks at 2 ⁇ angles selected from 4.3°, 8.3°, 8.6°, 13.0°, 14.0°, 15.9°, and 17.3°. In another embodiment, calcium salt crystalline Form II is characterized by at least six x-ray powder diffraction peaks at 2 ⁇ angles selected from 4.3°, 8.3°, 8.6°, 13.0°, 14.0°, 15.9°, and 17.3°. In another embodiment, calcium salt crystalline Form II is characterized by x-ray powder diffraction peaks at 2 ⁇ angles 4.3°, 8.3°, 8.6°, 13.0°, 14.0°, 15.9°, and 17.3°.
  • calcium salt crystalline Form II is characterized by at least three, four, five, six, or all x-ray powder diffraction peaks at 2 ⁇ angles selected from 4.3°, 8.3°, 8.6°, 13.0°, 14.0°, 15.9°, and 17.3°, and is further characterized by one or more x-ray powder diffraction peaks at 2 ⁇ angles selected from 10.8°, 14.9°, 18.4°, and 23.2°.
  • calcium salt crystalline Form II is characterized by one or more, or all of the x-ray powder diffraction peaks at 2 ⁇ angles provided in Table 23A.
  • calcium salt crystalline Form II is characterized by an x-ray powder diffraction substantially similar to Figure 11A.
  • calcium salt crystalline Form II is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 11A, or the peaks recited in Table 23A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 93.0 °C and 253.9 °C ⁇ 2 °C.
  • the molar ratio of calcium counter-ion to compound in calcium salt crystalline Form II is about 0.4
  • calcium salt crystalline Form II is further 29 ME1 ⁇ 53438692.v1 136867-00920 characterized by the features in any one of the previous two paragraphs, Figure 11A, or the peaks recited in Table 23A.
  • calcium salt crystalline Form II is an anhydrate, and is further characterized by the features in any one of the previous three paragraphs, Figure 11A, or the peaks recited in Table 23A.
  • Calcium Salt Form III In one embodiment, calcium salt crystalline Form III is characterized by at least three x-ray powder diffraction peaks at 2 ⁇ angles selected from 14.0°, 15.4°, 17.3°, 18.7°, 19.3°, 20.0°, and 22.8°. In another embodiment, calcium salt crystalline Form III is characterized by at least four x-ray powder diffraction peaks at 2 ⁇ angles selected from 14.0°, 15.4°, 17.3°, 18.7°, 19.3°, 20.0°, and 22.8°.
  • calcium salt crystalline Form III is characterized by at least five x-ray powder diffraction peaks at 2 ⁇ angles selected from 14.0°, 15.4°, 17.3°, 18.7°, 19.3°, 20.0°, and 22.8°. In another embodiment, calcium salt crystalline Form III is characterized by at least six x-ray powder diffraction peaks at 2 ⁇ angles selected from 14.0°, 15.4°, 17.3°, 18.7°, 19.3°, 20.0°, and 22.8°. In another embodiment, calcium salt crystalline Form III is characterized by x-ray powder diffraction peaks at 2 ⁇ angles 14.0°, 15.4°, 17.3°, 18.7°, 19.3°, 20.0°, and 22.8°.
  • calcium salt crystalline Form III is characterized by at least three, four, five, six, or all x-ray powder diffraction peaks at 2 ⁇ angles selected from 14.0°, 15.4°, 17.3°, 18.7°, 19.3°, 20.0°, and 22.8°, and is further characterized by one or more x-ray powder diffraction peaks at 2 ⁇ angles selected from 12.6°, 13.3°, 20.5°, and 24.0°.
  • calcium salt crystalline Form III is characterized by one or more, or all of the x-ray powder diffraction peaks at 2 ⁇ angles provided in Table 24A.
  • calcium salt crystalline Form III is characterized by an x-ray powder diffraction substantially similar to Figure 12A.
  • calcium salt crystalline Form III is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 12A, or the peaks recited in Table 24A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising a peak endotherm at 216.0 °C ⁇ 2 °C.
  • DSC differential scanning calorimeter
  • the molar ratio of calcium counter-ion to compound in calcium salt crystalline Form III is about 0.5
  • calcium salt crystalline Form III is further characterized by the features in any one of the previous two paragraphs, Figure 12A, or the peaks recited in Table 24A.
  • calcium salt crystalline Form III is a DMSO solvate, and is further characterized by the features in any one of the previous three paragraphs, Figure 12A, or the peaks recited in Table 24A.
  • Calcium Salt Form IV In one embodiment, calcium salt crystalline Form IV is characterized by at least three x-ray powder diffraction peaks at 2 ⁇ angles selected from 6.6°, 7.4°, 8.4°, 11.2°, 12.6°, 14.8°, 17.5°, 22.2°, and 23.3°.
  • calcium salt crystalline Form IV is characterized by at least four x-ray powder diffraction peaks at 2 ⁇ angles selected from 6.6°, 7.4°, 8.4°, 11.2°, 12.6°, 14.8°, 17.5°, 22.2°, and 23.3°.
  • calcium salt crystalline Form IV is characterized by at least five x-ray powder diffraction peaks at 2 ⁇ angles selected from 6.6°, 7.4°, 8.4°, 11.2°, 12.6°, 14.8°, 17.5°, 22.2°, and 23.3°.
  • calcium salt crystalline Form IV is characterized by at least six x-ray powder diffraction peaks at 2 ⁇ angles selected from 6.6°, 7.4°, 8.4°, 11.2°, 12.6°, 14.8°, 17.5°, 22.2°, and 23.3°.
  • calcium salt crystalline Form IV is characterized by at least seven x-ray powder diffraction peaks at 2 ⁇ angles selected from 6.6°, 7.4°, 8.4°, 11.2°, 12.6°, 14.8°, 17.5°, 22.2°, and 23.3°.
  • calcium salt crystalline Form IV is characterized by at least eight x-ray powder diffraction peaks at 2 ⁇ angles selected from 6.6°, 7.4°, 8.4°, 11.2°, 12.6°, 14.8°, 17.5°, 22.2°, and 23.3°.
  • calcium salt crystalline Form IV is characterized by x-ray powder diffraction peaks at 2 ⁇ angles 6.6°, 7.4°, 8.4°, 11.2°, 12.6°, 14.8°, 17.5°, 22.2°, and 23.3°.
  • calcium salt crystalline Form IV is characterized by at least three, four, five, six, seven, eight, or all x-ray powder diffraction peaks at 2 ⁇ angles selected from 6.6°, 7.4°, 8.4°, 11.2°, 12.6°, 14.8°, 17.5°, 22.2°, and 23.3°, and is further characterized by one or more x-ray powder diffraction peaks at 2 ⁇ angles selected from 13.6°, 16.8°, 21.1°, and 35.2°.
  • calcium salt crystalline Form IV is characterized by one or more, or all of the x-ray powder diffraction peaks at 2 ⁇ angles provided in Table 25A.
  • calcium salt crystalline Form IV is characterized by an x-ray powder diffraction substantially similar to Figure 13A.
  • calcium salt crystalline Form IV is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 13A, or the peaks recited in Table 25A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 65.7 °C, 123.1 °C, 174.7 °C and 186.4 °C ⁇ 2 °C.
  • DSC differential scanning calorimeter
  • the molar ratio of calcium counter-ion to compound in calcium salt crystalline Form IV is about 0.4, and calcium salt crystalline Form IV is further characterized by the features in any one of the previous two paragraphs, Figure 13A, or the peaks recited in Table 25A.
  • Calcium Salt Form V In one embodiment, calcium salt crystalline Form V is characterized by at least three x-ray powder diffraction peaks at 2 ⁇ angles selected from 6.4°, 7.0°, 12.5°, 13.9°, 17.5°, 23.3°, 25.6°, 26.4°, and 26.9°.
  • calcium salt crystalline Form V is characterized by at least four x-ray powder diffraction peaks at 2 ⁇ angles selected from 6.4°, 7.0°, 12.5°, 13.9°, 17.5°, 23.3°, 25.6°, 26.4°, and 26.9°.
  • calcium salt crystalline Form V is characterized by at least five x-ray powder diffraction peaks at 2 ⁇ angles selected from 6.4°, 7.0°, 12.5°, 13.9°, 17.5°, 23.3°, 25.6°, 26.4°, and 26.9°.
  • calcium salt crystalline Form V is characterized by at least six x-ray powder diffraction peaks at 2 ⁇ angles selected from 6.4°, 7.0°, 12.5°, 13.9°, 17.5°, 23.3°, 25.6°, 26.4°, and 26.9°.
  • calcium salt crystalline Form V is characterized by at least seven x-ray powder diffraction peaks at 2 ⁇ angles selected from 6.4°, 7.0°, 12.5°, 13.9°, 17.5°, 23.3°, 25.6°, 26.4°, and 26.9°.
  • calcium salt crystalline Form V is characterized by at least eight x-ray powder diffraction peaks at 2 ⁇ angles selected from 6.4°, 7.0°, 12.5°, 13.9°, 17.5°, 23.3°, 25.6°, 26.4°, and 26.9°.
  • calcium salt crystalline Form V is characterized by x-ray powder diffraction peaks at 2 ⁇ angles 6.4°, 7.0°, 12.5°, 13.9°, 17.5°, 23.3°, 25.6°, 26.4°, and 26.9°.
  • calcium salt crystalline Form V is characterized by at least three, four, five, six, seven, eight, or all x-ray powder diffraction peaks at 2 ⁇ angles selected from 6.4°, 7.0°, 12.5°, 13.9°, 17.5°, 23.3°, 25.6°, 26.4°, and 26.9°, and is further characterized by one or more x-ray powder diffraction peaks at 2 ⁇ angles selected from 7.7°, 9.3°, 15.4°, 21.1°, 22.2°, 24.6°, 28.8°, and 29.3°.
  • calcium salt crystalline Form V is characterized by one or more, or all of the x-ray powder diffraction peaks at 2 ⁇ angles provided in Table 25C.
  • calcium salt crystalline Form V is characterized by an x-ray powder diffraction substantially similar to Figure 14.
  • calcium salt crystalline Form V is a hydrate, and is further characterized any one of the sets of XRPD peaks of the previous paragraph, Figure 14, or the peaks recited in Table 25C.
  • 32 ME1 ⁇ 53438692.v1 136867-00920 Choline Salt Form I
  • choline salt crystalline Form I is characterized by at least three x- ray powder diffraction peaks at 2 ⁇ angles selected from 11.2°, 12.8°, 14.1°, 16.7°, 17.1°, 20.4°, 21.4°, and 28.4°.
  • choline salt crystalline Form I is characterized by at least four x-ray powder diffraction peaks at 2 ⁇ angles selected from 11.2°, 12.8°, 14.1°, 16.7°, 17.1°, 20.4°, 21.4°, and 28.4°. In another embodiment, choline salt crystalline Form I is characterized by at least five x-ray powder diffraction peaks at 2 ⁇ angles selected from 11.2°, 12.8°, 14.1°, 16.7°, 17.1°, 20.4°, 21.4°, and 28.4°.
  • choline salt crystalline Form I is characterized by at least six x-ray powder diffraction peaks at 2 ⁇ angles selected from 11.2°, 12.8°, 14.1°, 16.7°, 17.1°, 20.4°, 21.4°, and 28.4°. In another embodiment, choline salt crystalline Form I is characterized by at least seven x-ray powder diffraction peaks at 2 ⁇ angles selected from 11.2°, 12.8°, 14.1°, 16.7°, 17.1°, 20.4°, 21.4°, and 28.4°.
  • choline salt crystalline Form I is characterized by x-ray powder diffraction peaks at 2 ⁇ angles 11.2°, 12.8°, 14.1°, 16.7°, 17.1°, 20.4°, 21.4°, and 28.4°.
  • choline salt crystalline Form I is characterized by at least three, four, five, six, seven, or all x-ray powder diffraction peaks at 2 ⁇ angles selected from 11.2°, 12.8°, 14.1°, 16.7°, 17.1°, 20.4°, 21.4°, and 28.4°, and is further characterized by one or more x-ray powder diffraction peaks at 2 ⁇ angles selected from 16.4°, 18.9°, 22.5°, and 23.4°.
  • choline salt crystalline Form I is characterized by one or more, or all of the x-ray powder diffraction peaks at 2 ⁇ angles provided in Table 27A. In another embodiment, choline salt crystalline Form I is characterized by an x-ray powder diffraction substantially similar to Figure 15A. In another embodiment, choline salt crystalline Form I is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 15A, or the peaks recited in Table 27A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising a peak endotherm at 172.1 °C ⁇ 2 °C.
  • DSC differential scanning calorimeter
  • the molar ratio of choline counter-ion to compound in choline salt crystalline Form I is about 1.0, and choline salt crystalline Form I is further characterized by the features in any one of the previous two paragraphs, Figure 15A, or the peaks recited in Table 27A.
  • choline salt crystalline Form I is an anhydrate, and is further characterized by the features in any one of the previous three paragraphs, Figure 15A, or the peaks recited in Table 27A.
  • choline salt crystalline Form II is characterized by at least three x-ray powder diffraction peaks at 2 ⁇ angles selected from 6.6°, 9.9°, 10.9°, 13.3°, 20.0°, 21.4°, and 23.4°.
  • choline salt crystalline Form II is characterized by at least four x-ray powder diffraction peaks at 2 ⁇ angles selected from 6.6°, 9.9°, 10.9°, 13.3°, 20.0°, 21.4°, and 23.4°.
  • choline salt crystalline Form II is characterized by at least five x-ray powder diffraction peaks at 2 ⁇ angles selected from 6.6°, 9.9°, 10.9°, 13.3°, 20.0°, 21.4°, and 23.4°.
  • choline salt crystalline Form II is characterized by at least six x-ray powder diffraction peaks at 2 ⁇ angles selected from 6.6°, 9.9°, 10.9°, 13.3°, 20.0°, 21.4°, and 23.4°.
  • choline salt crystalline Form II is characterized by x-ray powder diffraction peaks at 2 ⁇ angles 6.6°, 9.9°, 10.9°, 13.3°, 20.0°, 21.4°, and 23.4°.
  • choline salt crystalline Form II is characterized by at least three, four, five, six, or all x-ray powder diffraction peaks at 2 ⁇ angles selected from 6.6°, 9.9°, 10.9°, 13.3°, 20.0°, 21.4°, and 23.4°, and is further characterized by one or more x-ray powder diffraction peaks at 2 ⁇ angles selected from 11.7°, 21.8°, 23.4°, and 27.5°.
  • choline salt crystalline Form II is characterized by one or more, or all of the x-ray powder diffraction peaks at 2 ⁇ angles provided in Table 28.
  • choline salt crystalline Form II is characterized by an x-ray powder diffraction substantially similar to Figure 16.
  • Choline Salt Form III In one embodiment, choline salt crystalline Form III is characterized by at least three x-ray powder diffraction peaks at 2 ⁇ angles selected from 7.4°, 11.1°, 14.8°, and 22.3°. In another embodiment, choline salt crystalline Form III is characterized by x-ray powder diffraction peaks at 2 ⁇ angles 7.4°, 11.1°, 14.8°, and 22.3°.
  • choline salt crystalline Form III is characterized by at least three, or all x-ray powder diffraction peaks at 2 ⁇ angles selected from 7.4°, 11.1°, 14.8°, and 22.3°, and is further characterized by one or more x-ray powder diffraction peaks at 2 ⁇ angles selected from 16.5°, 18.6°, 20.3°, and 33.4°.
  • choline salt crystalline Form III is characterized by one or more, or all of the x-ray powder diffraction peaks at 2 ⁇ angles provided in Table 29A.
  • choline salt crystalline Form III is characterized by an x-ray powder diffraction substantially similar to Figure 17A.
  • choline salt crystalline Form III is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 17A, or the peaks recited in 34 ME1 ⁇ 53438692.v1 136867-00920 Table 29A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 131.8 °C, and 175.7 °C, and a peak exotherm at 135.3 °C ⁇ 2 °C.
  • DSC differential scanning calorimeter
  • the molar ratio of choline counter-ion to compound in choline salt crystalline Form III is about 1.1, and choline salt crystalline Form III is further characterized by the features in any one of the previous two paragraphs, Figure 17A, or the peaks recited in Table 29A.
  • choline salt crystalline Form III is an anhydrate, and is further characterized by the features in any one of the previous three paragraphs, Figure 17A, or the peaks recited in Table 29A.
  • Choline Salt Form IV In one embodiment, choline salt crystalline Form IV is characterized by at least three x-ray powder diffraction peaks at 2 ⁇ angles selected from 10.5°, 13.3°, 17.4°, 18.3°, 20.7°, and 23.8°.
  • choline salt crystalline Form IV is characterized by at least four x-ray powder diffraction peaks at 2 ⁇ angles selected from 10.5°, 13.3°, 17.4°, 18.3°, 20.7°, and 23.8°. In another embodiment, choline salt crystalline Form IV is characterized by at least five x-ray powder diffraction peaks at 2 ⁇ angles selected from 10.5°, 13.3°, 17.4°, 18.3°, 20.7°, and 23.8°. In another embodiment, choline salt crystalline Form IV is characterized by x-ray powder diffraction peaks at 2 ⁇ angles 10.5°, 13.3°, 17.4°, 18.3°, 20.7°, and 23.8°.
  • choline salt crystalline Form IV is characterized by at least three, four, five, or all x-ray powder diffraction peaks at 2 ⁇ angles selected from 10.5°, 13.3°, 17.4°, 18.3°, 20.7°, and 23.8°, and is further characterized by one or more x-ray powder diffraction peaks at 2 ⁇ angles selected from 11.3°, 17.8°, 18.9°, 21.1°, 22.3°, 23.4°, and 24.3°.
  • choline salt crystalline Form IV is characterized by one or more, or all of the x-ray powder diffraction peaks at 2 ⁇ angles provided in Table 30A.
  • choline salt crystalline Form IV is characterized by an x-ray powder diffraction substantially similar to Figure 18A.
  • choline salt crystalline Form IV is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 18A, or the peaks recited in Table 30A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 116.4 °C, 142.3 °C, and 176.2 °C, and a peak exotherm at 144.6 °C ⁇ 2 °C.
  • DSC differential scanning calorimeter
  • the molar ratio of choline counter-ion to compound in choline salt crystalline Form IV is about 1.1, and choline salt crystalline Form IV is further characterized by the features in any one of the previous two paragraphs, Figure 18A, or the peaks recited in Table 30A.
  • choline salt crystalline Form IV is an EtOH solvate, and is further characterized by the features in any one of the previous three paragraphs, Figure 18A, or the peaks recited in Table 30A.
  • Choline Salt Form V is characterized by at least three x-ray powder diffraction peaks at 2 ⁇ angles selected from 10.6°, 14.5°, 17.4°, 18.6°, 20.7°, and 21.2°. In another embodiment, choline salt crystalline Form V is characterized by at least four x-ray powder diffraction peaks at 2 ⁇ angles selected from 10.6°, 14.5°, 17.4°, 18.6°, 20.7°, and 21.2°. In another embodiment, choline salt crystalline Form V is characterized by at least five x-ray powder diffraction peaks at 2 ⁇ angles selected from 10.6°, 14.5°, 17.4°, 18.6°, 20.7°, and 21.2°.
  • choline salt crystalline Form V is characterized by x-ray powder diffraction peaks at 2 ⁇ angles 10.6°, 14.5°, 17.4°, 18.6°, 20.7°, and 21.2°.
  • choline salt crystalline Form V is characterized by at least three, four, five, or all x-ray powder diffraction peaks at 2 ⁇ angles selected from 10.6°, 14.5°, 17.4°, 18.6°, 20.7°, and 21.2°, and is further characterized by one or more x-ray powder diffraction peaks at 2 ⁇ angles selected from 11.4°, 15.6°, 17.8°, 19.8°, and 24.2°.
  • choline salt crystalline Form V is characterized by one or more, or all of the x- ray powder diffraction peaks at 2 ⁇ angles provided in Table 31A. In another embodiment, choline salt crystalline Form V is characterized by an x-ray powder diffraction substantially similar to Figure 19A. In another embodiment, choline salt crystalline Form V is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 19A, or the peaks recited in Table 31A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 142.2 °C, and 176.3 °C, and a peak exotherm at 144.8 °C ⁇ 2 °C.
  • DSC differential scanning calorimeter
  • the molar ratio of choline counter-ion to compound in choline salt crystalline Form V is about 1.1, and choline salt crystalline Form V is further characterized by the features in any one of the previous two paragraphs, Figure 19A, or the peaks recited in Table 31A.
  • choline salt crystalline Form V is an anhydrate, and is further characterized by the features in any one of the previous three paragraphs, Figure 19A, or the peaks recited in Table 31A.
  • Choline Salt Form VI is characterized by at least three x-ray powder diffraction peaks at 2 ⁇ angles selected from 11.2°, 16.4°, 17.0°, 19.3°, 20.0°, 20.4°, and 22.9°. In another embodiment, choline salt crystalline Form VI is characterized by at least four x-ray powder diffraction peaks at 2 ⁇ angles selected from 11.2°, 16.4°, 17.0°, 19.3°, 20.0°, 20.4°, and 22.9°.
  • choline salt crystalline Form VI is characterized by at least five x-ray powder diffraction peaks at 2 ⁇ angles selected from 11.2°, 16.4°, 17.0°, 19.3°, 20.0°, 20.4°, and 22.9°.
  • choline salt crystalline Form VI is characterized by at least six x-ray powder diffraction peaks at 2 ⁇ angles selected from 11.2°, 16.4°, 17.0°, 19.3°, 20.0°, 20.4°, and 22.9°.
  • choline salt crystalline Form VI is characterized by x-ray powder diffraction peaks at 2 ⁇ angles 11.2°, 16.4°, 17.0°, 19.3°, 20.0°, 20.4°, and 22.9°.
  • choline salt crystalline Form VI is characterized by at least three, four, five, six, or all x-ray powder diffraction peaks at 2 ⁇ angles selected from 11.2°, 16.4°, 17.0°, 19.3°, 20.0°, 20.4°, and 22.9°, and is further characterized by one or more x-ray powder diffraction peaks at 2 ⁇ angles selected from 11.2°, 16.4°, 17.0°, 19.3°, 20.0°, 20.4°.
  • choline salt crystalline Form VI is characterized by one or more, or all of the x-ray powder diffraction peaks at 2 ⁇ angles provided in Table 32A.
  • choline salt crystalline Form VI is characterized by an x-ray powder diffraction substantially similar to Figure 20A.
  • choline salt crystalline Form VI is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 20A, or the peaks recited in Table 32A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising a peak endotherm at 174.6 °C ⁇ 2 °C.
  • DSC differential scanning calorimeter
  • the molar ratio of choline counter-ion to compound in choline salt crystalline Form VI is about 1.1, and choline salt crystalline Form VI is further characterized by the features in any one of the previous two paragraphs, Figure 20A, or the peaks recited in Table 32A.
  • choline salt crystalline Form VI is an anhydrate, and is further characterized by the features in any one of the previous three paragraphs, Figure 20A, or the peaks recited in Table 32A.
  • hydrogen bromide salt crystalline Form I is characterized by at least three x-ray powder diffraction peaks at 2 ⁇ angles selected from 4.8°, 8.7°, 15.2°, 17.7°, 24.1°, and 30.0°. In another embodiment, hydrogen bromide salt crystalline Form I is characterized by at least four x-ray powder diffraction peaks at 2 ⁇ angles selected from 4.8°, 8.7°, 15.2°, 17.7°, 24.1°, and 30.0°.
  • hydrogen bromide salt crystalline Form I is characterized by at least five x-ray powder diffraction peaks at 2 ⁇ angles selected from 4.8°, 8.7°, 15.2°, 17.7°, 24.1°, and 30.0°. In another embodiment, hydrogen bromide salt crystalline Form I is characterized by x-ray powder diffraction peaks at 2 ⁇ angles 4.8°, 8.7°, 15.2°, 17.7°, 24.1°, and 30.0°.
  • hydrogen bromide salt crystalline Form I is characterized by at least three, four, five, or all x-ray powder diffraction peaks at 2 ⁇ angles selected from 4.8°, 8.7°, 15.2°, 17.7°, 24.1°, and 30.0°, and is further characterized by one or more x-ray powder diffraction peaks at 2 ⁇ angles selected from 13.2°, 14.5°, 14.9°, and 15.8°.
  • hydrogen bromide salt crystalline Form I is characterized by one or more, or all of the x-ray powder diffraction peaks at 2 ⁇ angles provided in Table 34A.
  • hydrogen bromide salt crystalline Form I is characterized by an x-ray powder diffraction substantially similar to Figure 21A.
  • hydrogen bromide salt crystalline Form I is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 21A, or the peaks recited in Table 34A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 81.9 °C, 116.7 °C, 146.8 °C, and 169.7 °C ⁇ 2 °C.
  • the molar ratio of bromide counter-ion to compound in hydrogen bromide salt crystalline Form I is about 0.7
  • hydrogen bromide salt crystalline Form I is further characterized by the features in any one of the previous two paragraphs, Figure 21A, or the peaks recited in Table 34A.
  • hydrogen bromide salt crystalline Form II is characterized by at least three x-ray powder diffraction peaks at 2 ⁇ angles selected from 4.9°, 10.8°, 14.5°, 15.3°, 19.4°, 23.6°, and 24.2°.
  • hydrogen bromide salt crystalline Form II is characterized by at least four x-ray powder diffraction peaks at 2 ⁇ angles selected from 4.9°, 10.8°, 14.5°, 15.3°, 19.4°, 23.6°, and 24.2°.
  • hydrogen bromide salt 38 ME1 ⁇ 53438692.v1 136867-00920 crystalline Form II is characterized by at least five x-ray powder diffraction peaks at 2 ⁇ angles selected from 4.9°, 10.8°, 14.5°, 15.3°, 19.4°, 23.6°, and 24.2°.
  • hydrogen bromide salt crystalline Form II is characterized by at least six x-ray powder diffraction peaks at 2 ⁇ angles selected from 4.9°, 10.8°, 14.5°, 15.3°, 19.4°, 23.6°, and 24.2°.
  • hydrogen bromide salt crystalline Form II is characterized by x-ray powder diffraction peaks at 2 ⁇ angles 4.9°, 10.8°, 14.5°, 15.3°, 19.4°, 23.6°, and 24.2°.
  • hydrogen bromide salt crystalline Form II is characterized by at least three, four, five, six, or all x-ray powder diffraction peaks at 2 ⁇ angles selected from 4.9°, 10.8°, 14.5°, 15.3°, 19.4°, 23.6°, and 24.2°, and is further characterized by one or more x-ray powder diffraction peaks at 2 ⁇ angles selected from 6.8°, 9.7°, 15.6°, 17.4°, 21.6°, 29.2°, and 30.8°.
  • hydrogen bromide salt crystalline Form II is characterized by one or more, or all of the x-ray powder diffraction peaks at 2 ⁇ angles provided in Table 35A. In another embodiment, hydrogen bromide salt crystalline Form II is characterized by an x-ray powder diffraction substantially similar to Figure 22A. In another embodiment, hydrogen bromide salt crystalline Form II is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 22A, or the peaks recited in Table 35A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 111.2 °C and 147.8 °C ⁇ 2 °C.
  • DSC differential scanning calorimeter
  • the molar ratio of bromide counter-ion to compound in hydrogen bromide salt crystalline Form II is about 1.0, and hydrogen bromide salt crystalline Form II is further characterized by the features in any one of the previous two paragraphs, Figure 22A, or the peaks recited in Table 35A.
  • hydrogen bromide salt crystalline Form II is a hydrate, and is further characterized by the features in any one of the previous three paragraphs, Figure 22A, or the peaks recited in Table 35A.
  • hydrogen bromide salt crystalline Form III is characterized by at least three x-ray powder diffraction peaks at 2 ⁇ angles selected from 5.2°, 8.0°, 13.1°, 15.6°, 17.6°, 22.4°, and 28.9°.
  • hydrogen bromide salt crystalline Form III is characterized by at least four x-ray powder diffraction peaks at 2 ⁇ angles selected from 5.2°, 8.0°, 13.1°, 15.6°, 17.6°, 22.4°, and 28.9°.
  • hydrogen bromide salt crystalline Form III is characterized by at least five x-ray powder diffraction peaks at 2 ⁇ angles selected from 5.2°, 8.0°, 13.1°, 15.6°, 17.6°, 22.4°, and 28.9°.
  • 39 ME1 ⁇ 53438692.v1 136867-00920 hydrogen bromide salt crystalline Form III is characterized by at least six x-ray powder diffraction peaks at 2 ⁇ angles selected from 5.2°, 8.0°, 13.1°, 15.6°, 17.6°, 22.4°, and 28.9°.
  • hydrogen bromide salt crystalline Form III is characterized by one or more, or all of the x-ray powder diffraction peaks at 2 ⁇ angles provided in Table 36. In another embodiment, hydrogen bromide salt crystalline Form III is characterized by an x-ray powder diffraction substantially similar to Figure 23A.
  • 1,5-Naphthalenedisulfonate Salt Form I In one embodiment, 1,5-naphthalenedisulfonate salt crystalline Form I is characterized by at least three x-ray powder diffraction peaks at 2 ⁇ angles selected from 8.3°, 11.1°, 12.2°, 14.0°, 15.7°, and 16.0°.
  • 1,5-naphthalenedisulfonate salt crystalline Form I is characterized by at least four x-ray powder diffraction peaks at 2 ⁇ angles selected from 8.3°, 11.1°, 12.2°, 14.0°, 15.7°, and 16.0°. In another embodiment, 1,5- naphthalenedisulfonate salt crystalline Form I is characterized by at least five x-ray powder diffraction peaks at 2 ⁇ angles selected from 8.3°, 11.1°, 12.2°, 14.0°, 15.7°, and 16.0°.
  • 1,5-naphthalenedisulfonate salt crystalline Form I is characterized by x- ray powder diffraction peaks at 2 ⁇ angles 8.3°, 11.1°, 12.2°, 14.0°, 15.7°, and 16.0°.
  • 1,5-naphthalenedisulfonate salt crystalline Form I is characterized by at least three, four, five, or all x-ray powder diffraction peaks at 2 ⁇ angles selected from 8.3°, 11.1°, 12.2°, 14.0°, 15.7°, and 16.0°, and is further characterized by one or more x-ray powder diffraction peaks at 2 ⁇ angles selected from 7.5°, 13.1°, 14.5°, 15.0°, 16.4°, 16.7°, and 16.9°.
  • 1,5-naphthalenedisulfonate salt crystalline Form I is characterized by one or more, or all of the x-ray powder diffraction peaks at 2 ⁇ angles provided in Table 37A.
  • 1,5-naphthalenedisulfonate salt crystalline Form I is characterized by an x-ray powder diffraction substantially similar to Figure 24A.
  • 1,5-naphthalenedisulfonate salt crystalline Form I is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 24A, or the peaks recited in Table 37A, and is further characterized by a differential scanning 40 ME1 ⁇ 53438692.v1 136867-00920 calorimeter (DSC) thermogram comprising peak endotherms at 110.2 °C and 185.0 °C ⁇ 2 °C.
  • 1,5-naphthalenedisulfonate salt crystalline Form II is characterized by at least three x-ray powder diffraction peaks at 2 ⁇ angles selected from 5.9°, 13.2°, 18.2°, 18.6°, 23.2°, 25.8°, and 26.3°.
  • 1,5- naphthalenedisulfonate salt crystalline Form II is characterized by at least four x-ray powder diffraction peaks at 2 ⁇ angles selected from 5.9°, 13.2°, 18.2°, 18.6°, 23.2°, 25.8°, and 26.3°.
  • 1,5-naphthalenedisulfonate salt crystalline Form II is characterized by at least five x-ray powder diffraction peaks at 2 ⁇ angles selected from 5.9°, 13.2°, 18.2°, 18.6°, 23.2°, 25.8°, and 26.3°.
  • 1,5-naphthalenedisulfonate salt crystalline Form II is characterized by at least six x-ray powder diffraction peaks at 2 ⁇ angles selected from 5.9°, 13.2°, 18.2°, 18.6°, 23.2°, 25.8°, and 26.3°.
  • 1,5- naphthalenedisulfonate salt crystalline Form II is characterized by x-ray powder diffraction peaks at 2 ⁇ angles 5.9°, 13.2°, 18.2°, 18.6°, 23.2°, 25.8°, and 26.3°.
  • 1,5-naphthalenedisulfonate salt crystalline Form II is characterized by at least three, four, five, six, or all x-ray powder diffraction peaks at 2 ⁇ angles selected from 5.9°, 13.2°, 18.2°, 18.6°, 23.2°, 25.8°, and 26.3°, and is further characterized by one or more x-ray powder diffraction peaks at 2 ⁇ angles selected from 7.5°, 14.1°, 15.7°, and 22.5°.
  • 1,5-naphthalenedisulfonate salt crystalline Form II is characterized by one or more, or all of the x-ray powder diffraction peaks at 2 ⁇ angles provided in Table 38A.
  • 1,5-naphthalenedisulfonate salt crystalline Form II is characterized by an x-ray powder diffraction substantially similar to Figure 25A.
  • 1,5-naphthalenedisulfonate salt crystalline Form II is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 25A, or the peaks recited in Table 38A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 130.9 oC, 155.2 oC and 164.3 oC and a peak exotherm at 143.7 oC ⁇ 2 °C.
  • DSC differential scanning calorimeter
  • the molar ratio of 1,5-naphthalenedisulfonate counter-ion to compound in 1,5-naphthalenedisulfonate salt crystalline Form II is about 0.9, and 1,5- naphthalenedisulfonate salt crystalline Form II is further characterized by the features in any one of the previous two paragraphs, Figure 25A, or the peaks recited in Table 38A.
  • Edisylate Salt Form I In one embodiment, edisylate salt crystalline Form I is characterized by at least three x-ray powder diffraction peaks at 2 ⁇ angles selected from 13.3°, 14.3°, 14.8°, and 19.1°.
  • edisylate salt crystalline Form I is characterized by x-ray powder diffraction peaks at 2 ⁇ angles 13.3°, 14.3°, 14.8°, and 19.1°. In another embodiment, edisylate salt crystalline Form I is characterized by at least three, or all x-ray powder diffraction peaks at 2 ⁇ angles selected from 13.3°, 14.3°, 14.8°, and 19.1°, and is further characterized by one or more x-ray powder diffraction peaks at 2 ⁇ angles selected from 9.6°, 12.6°, 15.5°, and 17.3°.
  • edisylate salt crystalline Form I is characterized by one or more, or all of the x-ray powder diffraction peaks at 2 ⁇ angles provided in Table 39A. In another embodiment, edisylate salt crystalline Form I is characterized by an x-ray powder diffraction substantially similar to Figure 26A. In another embodiment, edisylate salt crystalline Form I is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 26A, or the peaks recited in Table 39A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 80.1 °C, 156.8 °C, and 170.5 °C ⁇ 2 °C.
  • DSC differential scanning calorimeter
  • the molar ratio of edisylate counter-ion to compound in edisylate salt crystalline Form I is about 0.8, and edisylate salt crystalline Form I is further characterized by the features in any one of the previous two paragraphs, Figure 26A, or the peaks recited in Table 37A.
  • Edisylate Salt Form II In one embodiment, edisylate salt crystalline Form II is characterized by at least three x-ray powder diffraction peaks at 2 ⁇ angles selected from 6.0°, 16.6°, 17.2°, 18.2°, 21.3°, 21.7°, and 22.4°.
  • edisylate salt crystalline Form II is characterized by at least four x-ray powder diffraction peaks at 2 ⁇ angles selected from 6.0°, 16.6°, 17.2°, 18.2°, 21.3°, 21.7°, and 22.4°.
  • edisylate salt crystalline Form II is characterized by at least five x-ray powder diffraction peaks at 2 ⁇ angles selected from 6.0°, 16.6°, 17.2°, 18.2°, 21.3°, 21.7°, and 22.4°.
  • edisylate salt crystalline Form II is characterized by at least six x-ray powder diffraction peaks at 2 ⁇ angles selected 42 ME1 ⁇ 53438692.v1 136867-00920 from 6.0°, 16.6°, 17.2°, 18.2°, 21.3°, 21.7°, and 22.4°.
  • edisylate salt crystalline Form II is characterized by x-ray powder diffraction peaks at 2 ⁇ angles 6.0°, 16.6°, 17.2°, 18.2°, 21.3°, 21.7°, and 22.4°.
  • edisylate salt crystalline Form II is characterized by at least three, four, five, six, or all x-ray powder diffraction peaks at 2 ⁇ angles selected from 6.0°, 16.6°, 17.2°, 18.2°, 21.3°, 21.7°, and 22.4°, and is further characterized by one or more x-ray powder diffraction peaks at 2 ⁇ angles selected from 13.5°, 17.5°, 19.1°, and 23.0°.
  • edisylate salt crystalline Form II is characterized by one or more, or all of the x-ray powder diffraction peaks at 2 ⁇ angles provided in Table 40A.
  • edisylate salt crystalline Form II is characterized by an x-ray powder diffraction substantially similar to Figure 27A.
  • edisylate salt crystalline Form II is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 27A, or the peaks recited in Table 40A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 74.2 oC, 116.5 oC and 131.1 oC and a peak exotherm at 143.7 oC ⁇ 2 °C.
  • DSC differential scanning calorimeter
  • the molar ratio of edisylate counter-ion to compound in edisylate salt crystalline Form II is about 0.8, and edisylate salt crystalline Form II is further characterized by the features in any one of the previous two paragraphs, Figure 27A, or the peaks recited in Table 40A.
  • Diethylamine Salt Form I In one embodiment, diethylamine salt crystalline Form I is characterized by at least three x-ray powder diffraction peaks at 2 ⁇ angles selected from 12.9°, 13.4°, 17.7°, 19.0°, 21.4°, 25.0°, and 30.0°.
  • diethylamine salt crystalline Form I is characterized by at least four x-ray powder diffraction peaks at 2 ⁇ angles selected from 12.9°, 13.4°, 17.7°, 19.0°, 21.4°, 25.0°, and 30.0°.
  • diethylamine salt crystalline Form I is characterized by at least five x-ray powder diffraction peaks at 2 ⁇ angles selected from 12.9°, 13.4°, 17.7°, 19.0°, 21.4°, 25.0°, and 30.0°.
  • diethylamine salt crystalline Form I is characterized by at least six x-ray powder diffraction peaks at 2 ⁇ angles selected from 12.9°, 13.4°, 17.7°, 19.0°, 21.4°, 25.0°, and 30.0°.
  • diethylamine salt crystalline Form I is characterized by x-ray powder diffraction peaks at 2 ⁇ angles 12.9°, 13.4°, 17.7°, 19.0°, 21.4°, 25.0°, and 30.0°.
  • diethylamine salt crystalline Form I is characterized by at least three, four, five, six, or all x- ray powder diffraction peaks at 2 ⁇ angles selected from 12.9°, 13.4°, 17.7°, 19.0°, 21.4°, 43 ME1 ⁇ 53438692.v1 136867-00920 25.0°, and 30.0°, and is further characterized by one or more x-ray powder diffraction peaks at 2 ⁇ angles selected from 8.7°, 13.2°, 14.9°, 15.1°, 15.8°, 17.0°, 20.3°, 21.1°, and 23.4°.
  • diethylamine salt crystalline Form I is characterized by one or more, or all of the x-ray powder diffraction peaks at 2 ⁇ angles provided in Table 41A. In another embodiment, diethylamine salt crystalline Form I is characterized by an x-ray powder diffraction substantially similar to Figure 28A. In another embodiment, diethylamine salt crystalline Form I is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 28A, or the peaks recited in Table 41A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 98.7 °C and 195.9 °C ⁇ 2 °C.
  • DSC differential scanning calorimeter
  • diethylamine salt crystalline Form II is characterized by at least three x-ray powder diffraction peaks at 2 ⁇ angles selected from 3.7°, 7.3°, 11.0°, 12.3°, 13.8°, 14.6°, 16.9°, and 17.9°.
  • diethylamine salt crystalline Form II is characterized by at least four x-ray powder diffraction peaks at 2 ⁇ angles selected from 3.7°, 7.3°, 11.0°, 12.3°, 13.8°, 14.6°, 16.9°, and 17.9°.
  • diethylamine salt crystalline Form II is characterized by at least five x-ray powder diffraction peaks at 2 ⁇ angles selected from 3.7°, 7.3°, 11.0°, 12.3°, 13.8°, 14.6°, 16.9°, and 17.9°.
  • diethylamine salt crystalline Form II is characterized by at least six x-ray powder diffraction peaks at 2 ⁇ angles selected from 3.7°, 7.3°, 11.0°, 12.3°, 13.8°, 14.6°, 16.9°, and 17.9°.
  • diethylamine salt crystalline Form II is characterized by at least seven x-ray powder diffraction peaks at 2 ⁇ angles selected from 3.7°, 7.3°, 11.0°, 12.3°, 13.8°, 14.6°, 16.9°, and 17.9°.
  • diethylamine salt crystalline Form II is characterized by x-ray powder diffraction peaks at 2 ⁇ angles 3.7°, 7.3°, 11.0°, 12.3°, 13.8°, 14.6°, 16.9°, and 17.9°.
  • diethylamine salt crystalline Form II is characterized by at least three, four, five, six, seven, or all x-ray powder diffraction peaks at 2 ⁇ angles selected from 3.7°, 7.3°, 11.0°, 12.3°, 13.8°, 14.6°, 16.9°, and 17.9°, and is further characterized by one or more x-ray powder diffraction peaks at 2 ⁇ angles selected from 8.5°, 10.3°, 18.2°, 20.9°, and 22.9°.
  • diethylamine salt 44 ME1 ⁇ 53438692.v1 136867-00920 crystalline Form II is characterized by one or more, or all of the x-ray powder diffraction peaks at 2 ⁇ angles provided in Table 42A.
  • diethylamine salt crystalline Form II is characterized by an x-ray powder diffraction substantially similar to Figure 29A.
  • diethylamine salt crystalline Form II is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 29A, or the peaks recited in Table 42A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 119.8 oC, 180.0 oC and 192.0 oC.
  • the molar ratio of diethylamine counter-ion to compound in diethylamine salt crystalline Form II is about 0.9
  • diethylamine salt crystalline Form II is further characterized by the features in any one of the previous two paragraphs, Figure 29A, or the peaks recited in Table 42A.
  • hydrogen chloride salt crystalline Form I is characterized by at least three x-ray powder diffraction peaks at 2 ⁇ angles selected from 4.8°, 6.8°, 14.4°, 15.3°, 19.4°, and 24.1°. In another embodiment, hydrogen chloride salt crystalline Form I is characterized by at least four x-ray powder diffraction peaks at 2 ⁇ angles selected from 4.8°, 6.8°, 14.4°, 15.3°, 19.4°, and 24.1°. In another embodiment, hydrogen chloride salt crystalline Form I is characterized by at least five x-ray powder diffraction peaks at 2 ⁇ angles selected from 4.8°, 6.8°, 14.4°, 15.3°, 19.4°, and 24.1°.
  • hydrogen chloride salt crystalline Form I is characterized by x-ray powder diffraction peaks at 2 ⁇ angles 4.8°, 6.8°, 14.4°, 15.3°, 19.4°, and 24.1°.
  • hydrogen chloride salt crystalline Form I is characterized by at least three, four, five, or all x-ray powder diffraction peaks at 2 ⁇ angles selected from 4.8°, 6.8°, 14.4°, 15.3°, 19.4°, and 24.1°, and is further characterized by one or more x-ray powder diffraction peaks at 2 ⁇ angles selected from 9.7°, 15.9°, 21.7°, 29.2°, and 30.9°.
  • hydrogen chloride salt crystalline Form I is characterized by one or more, or all of the x-ray powder diffraction peaks at 2 ⁇ angles provided in Table 43A. In another embodiment, hydrogen chloride salt crystalline Form I is characterized by an x-ray powder diffraction substantially similar to Figure 30A.
  • hydrogen chloride salt crystalline Form I is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 30A, or the peaks recited in Table 43A, and is further characterized by a differential scanning calorimeter 45 ME1 ⁇ 53438692.v1 136867-00920 (DSC) thermogram comprising peak endotherms at 93.9 oC, 137.6 oC, 153.4 oC, and 166.7 oC ⁇ 2 °C.
  • DSC differential scanning calorimeter 45
  • the molar ratio of chloride counter-ion to compound in hydrogen chloride salt crystalline Form I is about 0.6, and hydrogen chloride salt crystalline Form I is further characterized by the features in any one of the previous two paragraphs, Figure 30A, or the peaks recited in Table 43A.
  • HCl Salt Form II In one embodiment, hydrogen chloride salt crystalline Form II is characterized by at least three x-ray powder diffraction peaks at 2 ⁇ angles selected from 4.8°, 8.7°, 13.3°, 17.8°, 24.1°, 29.0°, and 30.0°.
  • hydrogen chloride salt crystalline Form II is characterized by at least four x-ray powder diffraction peaks at 2 ⁇ angles selected from 4.8°, 8.7°, 13.3°, 17.8°, 24.1°, 29.0°, and 30.0°.
  • hydrogen chloride salt crystalline Form II is characterized by at least five x-ray powder diffraction peaks at 2 ⁇ angles selected from 4.8°, 8.7°, 13.3°, 17.8°, 24.1°, 29.0°, and 30.0°.
  • hydrogen chloride salt crystalline Form II is characterized by at least six x-ray powder diffraction peaks at 2 ⁇ angles selected from 4.8°, 8.7°, 13.3°, 17.8°, 24.1°, 29.0°, and 30.0°.
  • hydrogen chloride salt crystalline Form II is characterized by x-ray powder diffraction peaks at 2 ⁇ angles 4.8°, 8.7°, 13.3°, 17.8°, 24.1°, 29.0°, and 30.0°.
  • hydrogen chloride salt crystalline Form II is characterized by at least three, four, five, six, or all x-ray powder diffraction peaks at 2 ⁇ angles selected from 4.8°, 8.7°, 13.3°, 17.8°, 24.1°, 29.0°, and 30.0°, and is further characterized by one or more x-ray powder diffraction peaks at 2 ⁇ angles selected from 5.4°, 9.6°, 12.4°, 14.4°, 19.2°, and 33.9°.
  • hydrogen chloride salt crystalline Form II is characterized by one or more, or all of the x-ray powder diffraction peaks at 2 ⁇ angles provided in Table 44.
  • hydrogen chloride salt crystalline Form II is characterized by an x-ray powder diffraction substantially similar to Figure 31.
  • HCl Salt Form III hydrogen chloride salt crystalline Form III is characterized by at least three x-ray powder diffraction peaks at 2 ⁇ angles selected from 4.8°, 6.3°, 8.7°, 14.2°, 16.5°, 23.5°, and 24.1°.
  • hydrogen chloride salt crystalline Form III is characterized by at least four x-ray powder diffraction peaks at 2 ⁇ angles selected from 4.8°, 6.3°, 8.7°, 14.2°, 16.5°, 23.5°, and 24.1°.
  • hydrogen chloride salt crystalline Form III is characterized by at least five x-ray powder diffraction peaks at 2 ⁇ 46 ME1 ⁇ 53438692.v1 136867-00920 angles selected from 4.8°, 6.3°, 8.7°, 14.2°, 16.5°, 23.5°, and 24.1°.
  • hydrogen chloride salt crystalline Form III is characterized by at least six x-ray powder diffraction peaks at 2 ⁇ angles selected from 4.8°, 6.3°, 8.7°, 14.2°, 16.5°, 23.5°, and 24.1°.
  • hydrogen chloride salt crystalline Form III is characterized by x-ray powder diffraction peaks at 2 ⁇ angles 4.8°, 6.3°, 8.7°, 14.2°, 16.5°, 23.5°, and 24.1°.
  • hydrogen chloride salt crystalline Form III is characterized by at least three, four, five, six, or all x-ray powder diffraction peaks at 2 ⁇ angles selected from 4.8°, 6.3°, 8.7°, 14.2°, 16.5°, 23.5°, and 24.1°, and is further characterized by one or more x-ray powder diffraction peaks at 2 ⁇ angles selected from 8.1°, 19.2°, 20.3°, 25.1°, and 30.0°.
  • hydrogen chloride salt crystalline Form III is characterized by one or more, or all of the x-ray powder diffraction peaks at 2 ⁇ angles provided in Table 45. In another embodiment, hydrogen chloride salt crystalline Form III is characterized by an x-ray powder diffraction substantially similar to Figure 32.
  • HCl Salt Form IV In one embodiment, hydrogen chloride salt crystalline Form IV is characterized by at least three x-ray powder diffraction peaks at 2 ⁇ angles selected from 4.8°, 8.7°, 13.2°, 13.3°, 15.8°, 17.7°, 21.1°, and 30.0°.
  • hydrogen chloride salt crystalline Form IV is characterized by at least four x-ray powder diffraction peaks at 2 ⁇ angles selected from 4.8°, 8.7°, 13.2°, 13.3°, 15.8°, 17.7°, 21.1°, and 30.0°.
  • hydrogen chloride salt crystalline Form IV is characterized by at least five x-ray powder diffraction peaks at 2 ⁇ angles selected from 4.8°, 8.7°, 13.2°, 13.3°, 15.8°, 17.7°, 21.1°, and 30.0°.
  • hydrogen chloride salt crystalline Form IV is characterized by at least six x-ray powder diffraction peaks at 2 ⁇ angles selected from 4.8°, 8.7°, 13.2°, 13.3°, 15.8°, 17.7°, 21.1°, and 30.0°.
  • hydrogen chloride salt crystalline Form IV is characterized by at least seven x-ray powder diffraction peaks at 2 ⁇ angles selected from 4.8°, 8.7°, 13.2°, 13.3°, 15.8°, 17.7°, 21.1°, and 30.0°.
  • hydrogen chloride salt crystalline Form IV is characterized by x-ray powder diffraction peaks at 2 ⁇ angles 4.8°, 8.7°, 13.2°, 13.3°, 15.8°, 17.7°, 21.1°, and 30.0°.
  • hydrogen chloride salt crystalline Form IV is characterized by at least three, four, five, six, seven, or all x-ray powder diffraction peaks at 2 ⁇ angles selected from 4.8°, 8.7°, 13.2°, 13.3°, 15.8°, 17.7°, 21.1°, and 30.0°, and is further characterized by one or more x-ray powder diffraction peaks at 2 ⁇ angles selected from 5.4°, 14.2°, 14.9°, 16.2°, 17.4° and 19.6°.
  • hydrogen chloride salt crystalline Form IV is characterized by one or 47 ME1 ⁇ 53438692.v1 136867-00920 more, or all of the x-ray powder diffraction peaks at 2 ⁇ angles provided in Table 46A.
  • hydrogen chloride salt crystalline Form IV is characterized by an x-ray powder diffraction substantially similar to Figure 33A.
  • hydrogen chloride salt crystalline Form IV is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 33A, or the peaks recited in Table 46A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising a peak endotherm at 178.5 oC, and peak exotherms at 91.6 oC and 160.2 oC.
  • DSC differential scanning calorimeter
  • the molar ratio of chloride counter-ion to compound in hydrogen chloride salt crystalline Form IV is about 0.3, and hydrogen chloride salt crystalline Form IV is further characterized by the features in any one of the previous two paragraphs, Figure 33A, or the peaks recited in Table 46A.
  • pharmaceutical compositions comprising any of one the crystalline salt Forms described herein.
  • the pharmaceutical composition comprises a pharmaceutically acceptable carrier and any of the crystalline salt Forms as described herein.
  • the pharmaceutical composition comprises at least one solid pharmaceutically acceptable carrier and any of the crystalline salt Forms as described herein.
  • “Pharmaceutically acceptable carrier” refers to a substance that aids the formulation and/or administration of an active agent to and/or absorption by a subject and can be included in the compositions of the present disclosure without causing a significant adverse toxicological effect on the subject.
  • Non-limiting examples of pharmaceutically acceptable carriers include water, NaCl, normal saline solutions, lactated Ringer’s, normal sucrose, normal glucose, binders, fillers, disintegrants, lubricants, coatings, sweeteners, flavors, salt solutions (such as Ringer’s solution), alcohols, oils, gelatins, carbohydrates such as lactose, amylose or starch, hydroxymethycellulose, fatty acid esters, polyvinyl pyrrolidine, and colors, and the like.
  • Such preparations can be sterilized and, if desired, mixed with auxiliary agents such as lubricants, preservatives, stabilizers, wetting agents, emulsifiers, salts for influencing osmotic pressure, buffers, coloring, and/or aromatic substances and the like that do not deleteriously react with or interfere with the activity of the compounds provided herein.
  • auxiliary agents such as lubricants, preservatives, stabilizers, wetting agents, emulsifiers, salts for influencing osmotic pressure, buffers, coloring, and/or aromatic substances and the like that do not deleteriously react with or interfere with the activity of the compounds provided herein.
  • auxiliary agents such as lubricants, preservatives, stabilizers, wetting agents, emulsifiers, salts for influencing osmotic pressure, buffers, coloring, and/or aromatic substances and the like that do not deleteriously react with or interfere with the activity of the compounds provided herein.
  • compositions described herein optionally include one or more pharmaceutically acceptable carriers such as lactose, starch, cellulose and dextrose.
  • pharmaceutically acceptable carriers such as lactose, starch, cellulose and dextrose.
  • Other excipients such as flavoring agents, sweeteners, and preservatives, such as methyl, ethyl, propyl and butyl parabens, can also be included. More complete listings of suitable excipients can be found in the Handbook of Pharmaceutical Excipients (5 th Ed., Pharmaceutical Press (2005)). A person skilled in the art would know how to prepare formulations suitable for various types of administration routes.
  • Suitable formulations are described, for example, in Remington's Pharmaceutical Sciences (2003 - 20th edition) and in The United States Pharmacopeia: The National Formulary (USP 24 NF19) published in 1999.
  • the carriers, diluents and/or excipients are “acceptable” in the sense of being compatible with the other ingredients of the pharmaceutical composition and not deleterious to the recipient thereof.
  • MEK mitogen-activated protein kinase
  • ERK extra cellular signal-regulated kinases
  • a “subject” is a mammal in need of treatment.
  • the mammal can be a veterinary animal (e.g., dog or cat, and the like), farm animal (e.g., horse, cow, sheep or goat and the like) or laboratory animal (e.g., mouse, rat or guinea pig and the like). Most commonly, the subject is a human.
  • a “subject in need of treatment” is a subject with a disease in which medical treatment is desirable. In some embodiments, the disease is cancer.
  • the cancer is selected from breast cancer, prostate cancer, esophageal cancer, colon cancer, endometrial cancer, blood cancer, brain cancer, glioma, head and neck cancer, thyroid cancer, gallbladder cancer, bladder cancer, skin cancer, malignant melanoma, cancer of the uterus, cancer of the ovary, lung cancer, pancreatic cancer, liver cancer, renal cancer, testicular cancer, renal pelvic and ureteral cancer, prostate cancer, gastric cancer, stomach cancer, and hematological cancer.
  • the lung cancer is selected from non-small cell lung cancer, small cell lung cancer, and lung carcinoid tumor.
  • the head and neck 49 ME1 ⁇ 53438692.v1 136867-00920 cancer is selected from pharyngeal cancer, laryngeal cancer, tongue cancer, and the like.
  • the hematological cancer is selected from leukemia, lymphoma, and multiple myeloma.
  • the hematological cancer is acute myeloblastic leukemia, chronic myeloid leukemia, B cell lymphoma, chronic lymphocytic leukemia (CLL), Non- Hodgkins lymphoma, hairy cell leukemia, Mantle cell lymphoma, Burkitt lymphoma, small lymphocytic lymphoma, follicular lymphoma, lymphoplasmacytic lymphoma, extranodal marginal zone lymphoma, activated B-cell like (ABC) diffuse large B cell lymphoma, or germinal center B cell (GCB) diffuse large B cell lymphoma.
  • BCBC activated B-cell like
  • GCB germinal center B cell
  • the leukemia is selected from acute lymphoblastic leukemia (ALL), chronic lymphocytic leukemia (CLL), acute myelogenous leukemia (AML), acute myelocytic leukemia, acute lymphocytic leukemia, chronic myeloid leukemia (CML), chronic myelocytic leukemia, chronic lymphocytic leukemia, hairy cell leukemia, T-cell prolymphocytic leukemia, juvenile myelomonocytic leukemia, myelodysplastic syndrome, and follicular lymphoma.
  • the lymphoma is Hodgkin’s lymphoma or non-Hodgkin’s lymphoma (NHL).
  • the non-Hodgkin lymphoma is selected from relapsed NHL, refractory NHL, and recurrent follicular NHL.
  • the cancer is characterized by an NRAS mutation.
  • the cancer is characterized by an NRAS mutation at position 61 (i.e., Q61X, where X is a naturally occurring amino acid).
  • the cancer is characterized by an NRAS Q61R, NRAS Q61L, NRAS Q61K, NRAS Q61P or NRAS Q61H mutation.
  • the cancer is characterized by an NRAS Q61R, NRAS Q61L, NRAS Q61K, NRAS Q61P or NRAS Q61H mutation and is a cancer of the bladder/urinary tract, lung, skin, liver, myeloid, lymphoid, ovarian/fallopian tube, peripheral nervous system, soft tissue or vulva/vagina.
  • the cancer is of the bladder/urinary tract, lung or skin, each characterized by an NRAS Q61R mutation; cancer of the liver, myeloid, skin, lymphoid or bladder/urinary tract, each characterized by an NRAS Q61L mutation; cancer of the lung, lymphoid, ovarian/fallopian tube, peripheral nervous system, soft tissue, vulva/vagina, liver or skin, each characterized by an NRAS Q61K mutation; cancer of the myeloid characterized by an NRAS Q61P mutation; or cancer of the soft tissue characterized by an NRAS Q61H mutation.
  • the cancer is 50 ME1 ⁇ 53438692.v1 136867-00920 characterized by an NRAS Q61R, NRAS Q61L, NRAS Q61K, NRAS Q61P or NRAS Q61H and is bladder urothelial carcinoma, non-small cell lung cancer, melanoma, hepatoblastoma, acute myeloid leukemia, non-hodgkin lymphoma, ovarian epithelial tumor, neuroblastoma, fibrosarcoma, mucosal melanoma of the vulva/vagina, hepatocellular carcinoma or rhabdomyosarcoma.
  • the cancer is characterized by an NRAS Q61R mutation, and is bladder urothelial carcinoma, non-small cell lung cancer or melanoma.
  • the cancer is characterized by an NRAS Q61L mutation, and is hepatoblastoma, acute myeloid leukemia, melanoma, non-hodgkin lymphoma or bladder urothelial carcinoma.
  • the cancer is characterized by an NRAS Q61K mutation, and is non-small cell lung cancer, non-hodgkin lymphoma, ovarian epithelial tumor, neuroblastoma, melanoma, fibrosarcoma, mucosal melanoma of the vulva/vagina or hepatocellular carcinoma.
  • the cancer is characterized by an NRAS Q61P mutation, and is acute myeloid leukemia.
  • the cancer is characterized by an NRAS Q61H mutation, and is rhabdomyosarcoma.
  • the cancer is characterized by an NRAS A91V or E132K mutation.
  • the cancer is characterized by an NRAS A91V or E132K mutation and is from the bowel, e.g., the cancer is colorectal adenocarcinoma.
  • the cancer is characterized by an NRAS T20 frame shift deletion.
  • the cancer is characterized by an NRAS T20 frame shift deletion and is from the lung, e.g., the cancer is lung neuroendocrine tumor.
  • the cancer is characterized by an NRAS G12C, G12V, G12D, G12A, G12S or G12R mutation.
  • the cancer is characterized by an NRAS G12C, G12V, G12D, G12A, G12S or G12R mutation and is a cancer from myeloid, skin, lymphoid or ovary/fallopian tubes.
  • the cancer is characterized by an NRAS G12C mutation and is from myeloid.
  • the cancer is characterized by an NRAS G12V mutation and is from skin.
  • the cancer is characterized by an NRAS G12D mutation and is from lymphoid, myeloid and ovaries/fallopian tubes.
  • the cancer is characterized by an NRAS G12R mutation and is from myeloid.
  • the cancer is characterized by an NRAS G12C, G12V, G12D, G12A, G12S or G12R mutation and is acute myeloid leukemia, non-hodgkins lymphoma, melanoma or ovarian epithelial tumor.
  • the cancer is characterized by an NRAS G12C mutation and is acute myeloid leukemia.
  • the cancer is characterized by an NRAS G12V mutation 51 ME1 ⁇ 53438692.v1 136867-00920 and is melanoma.
  • the cancer is characterized by an NRAS G12D mutation and is acute myeloid leukemia, non-hodgkins lympohoma or ovarian epithelial tumor.
  • the cancer is characterized by an NRAS G12R mutation and is acute myeloid leukemia.
  • the cancer is characterized by an NRAS G13D or NRAS G13R mutation.
  • the cancer is characterized by an NRAS G13D or NRAS G13R mutation and is a cancer of the myeloid, lymphoid or skin.
  • the cancer is characterized by an NRAS G13D mutation and is a cancer from lymphoid (e.g., non-hodgkin lymphoma).
  • the cancer is characterized by an NRAS G13R mutation and is a cancer from myeloid (e.g., acute myeloid leukemia) or skin (e.g., melanoma).
  • the cancer is characterized by a KRAS mutation.
  • the cancer is characterized by an KRAS mutation at position 13 (i.e., G13X, where X is a naturally occurring amino acid).
  • the cancer is characterized by a KRAS G13D, KRAS G13C or KRAS G13V mutation.
  • the cancer is characterized by a KRAS G13D, KRAS G13C or KRAS G13V mutation and is a cancer of the bowel, lung, breast.
  • the cancer is characterized by a KRAS G13D mutation and is of the bowel, lung or breast; or by a KRAS G13C mutation and is of the lung.
  • the cancer is characterized by a KRAS G13D or KRAS G13C mutation and is colorectal carcinoma, non-small lung cell cancer or invasive breast carcinoma.
  • the cancer is characterized by a KRAS mutation at V14L, V9I, I187V, A59T, P140H, A146T, L19F, A18D, A146V, K117N, P121H, A59G, V160A.
  • the cancer is lymphoid characterized by a KRAS mutation at V14L or V9I.
  • the cancer is bone characterized by a KRAS mutation at I187V or A59T.
  • the cancer is bowel characterized by a KRAS mutation at P140H or A146T.
  • the cancer is lung characterized by a KRAS mutation at L19F.
  • the cancer is myeloid characterized by a KRAS mutation at A18D, A146V or K117N.
  • the cancer is ovary/fallopian tube characterized by a KRAS mutation at P121H or A59G.
  • the cancer is uterus characterized by a KRAS mutation at V160A.
  • the cancer is characterized by a KRAS mutation at V14L and is B-lymphoblastic leukemia/lymphoma.
  • the cancer is characterized by a KRAS 52 ME1 ⁇ 53438692.v1 136867-00920 mutation at V9I and is non-hodgkin lymphoma.
  • the cancer is characterized by a KRAS mutation at I187V or A59T and is osteosarcoma. In another embodiment, the cancer is characterized by a KRAS mutation at P140H or A146T and is colorectal adenocarcinoma. In another embodiment, the cancer is characterized by a KRAS mutation at L19F and is non-small cell lung cancer. In another embodiment, the cancer is characterized by a KRAS mutation at A18D, A146V or K117N and is acute myeloid leukemia. In another embodiment, the cancer is characterized by a KRAS mutation at P121H or A59G and is ovarian epithelial tumor.
  • the cancer is characterized by a KRAS mutation at V160A and is endometrial carcinoma.
  • the cancer is characterized by an KRAS mutation at position 12 (i.e., G12X, where X is a naturally occurring amino acid).
  • the cancer is characterized by a KRAS G12D, G12V, G12A, G12R, G12S or G12C mutation.
  • the cancer is characterized by a KRAS G12D, G12V, G12A, G12R, G12S or G12C mutation and is a cancer of the bowel, esophagus/stomach, ovary/fallopian tube, pancreas, uterus, lung, soft tissue, biliary tract, breast, lymphoid, thyroid or cervix.
  • the cancer is characterized by a KRAS G12D mutation and is a cancer of the bowel, esophagus/stomach, ovary/fallopian tube, pancreas, uterus or lung,
  • the cancer is characterized by a KRAS G12V mutation and is a cancer of the bowel, lung, pancreas, uterus, soft tissue, biliary tract or breast.
  • the cancer is characterized by a KRAS G12A mutation and is a cancer of the lymphoid, lung or bowel.
  • the cancer is characterized by a KRAS G12R mutation and is a cancer of the thyroid or pancreas.
  • the cancer is characterized by a KRAS G12S mutation and is a cancer of the lungs or bowel. In another embodiment, the cancer is characterized by a KRAS G12C mutation and is a cancer of the bowel, lung, cervix, esophagus/stomach or pancreas.
  • the cancer is characterized by a KRAS G12D, G12V, G12A, G12R, G12S or G12C mutation and is colorectal adenocarcinoma, esophagogastric adenocarcinoma, ovarian epithelial tumor, pancreatic adenocarcinoma, endometrial carcinoma, non-small cell lung cancer, lung neuroendocrine tumor, leiomyosarcoma, intraductal papillary neoplasm of the bile duct, invasive breast carcinoma, non-hodgkin lymphoma, anaplastic thyroid cancer, cervical squamous cell carcinoma or esophageal squamous cell carcinoma.
  • the cancer is characterized by a KRAS G12D and is colorectal adenocarcinoma, esophagogastric adenocarcinoma, ovarian epithelial 53 ME1 ⁇ 53438692.v1 136867-00920 tumor, pancreatic adenocarcinoma, endometrial carcinoma or non-small cell lung cancer.
  • the cancer is characterized by a KRAS G12V mutation and is colorectal adenocarcinoma, non-small cell lung cancer, lung neuroendocrine tumor, pancreatic adenocarcinoma, endometrial carcinoma, leiomyosarcoma, intraductal papillary neoplasm of the bile duct or invasive breast carcinoma.
  • the cancer is characterized by a KRAS G12A mutation and is colorectal adenocarcinoma, non-hodgkin lymphoma or non-small cell lung cancer.
  • the cancer is characterized by a KRAS G12R mutation and is anaplastic thyroid cancer or pancreatic adenocarcinoma.
  • the cancer is characterized by a KRAS G12S mutation and is non-small cell lung cancer or colorectal adenocarincoma.
  • the cancer is characterized by an KRAS mutation at position 61 (i.e., Q61X, where X is a naturally occurring amino acid).
  • the cancer is characterized by a KRAS Q61H, Q61L, Q61K, Q61R, Q61P or G61E mutation.
  • the cancer is characterized by a KRAS Q61H, Q61L, Q61K, Q61R, Q61P or Q61E mutation and are cancers of the bowel, pancreas or lung.
  • the cancer is characterized by a Q61H KRAS mutation and is a cancer of the bowel or pancreas. In another embodiment, the cancer is characterized by a KRAS Q61L mutation and is a cancer of the bowel. In another embodiment, the cancer is characterized by a KRAS Q61K and is a cancer of the lung. In another embodiment, the cancer is characterized by a KRAS Q61R and is a cancer of the lung. In another embodiment, the cancer is characterized by a KRAS Q61H, Q61L, Q61K, Q61R, Q61P or G61E mutation and is colorectal adenocarcinoma, pancreatic adenocarcinoma or non-small cell lung cancer.
  • the cancer is characterized by a KRAS Q61R and is non-small cell lung cancer.
  • the cancer is characterized by a KRAS Q61H mutation and is colorectal adenocarcinoma or pancreatic adenocarcinoma.
  • the cancer is characterized by a KRAS Q61L mutation and is colorectal adenocarcinoma.
  • the cancer is characterized by a KRAS Q61K mutation and is non-small cell lung cancer.
  • a subject with one of the aforementioned cancers may be treated by administering to the subject an effective amount of any one of crystalline salt Forms as described herein, or a pharmaceutical composition thereof.
  • the methods comprise administering an effective amount of a any one of crystalline salt Forms as described herein, or a pharmaceutical composition 54 ME1 ⁇ 53438692.v1 136867-00920 thereof, in combination with an effective amount of an anticancer agent, wherein the amounts of the combination and the chemotherapeutic are together effective in treating a subject with cancer.
  • chemotherapeutics are presently known in the art and can be used in combination.
  • the chemotherapeutic is selected from mitotic inhibitors, alkylating agents, anti-metabolites, intercalating antibiotics, growth factor inhibitors, cell cycle inhibitors, enzymes, topoisomerase inhibitors, biological response modifiers, anti- hormones, angiogenesis inhibitors, and anti- androgens.
  • methods for treating a subject with cancer comprising administering to the mammal an amount of a MEK protein kinase inhibitor and/or Raf protein kinase inhibitor in combination with radiation therapy, wherein the amounts of the MEK protein kinase inhibitor and/or Raf protein kinase inhibitor in combination with the radiation therapy effective in treating a subject with cancer.
  • the disclosure also relates to a method of inhibiting abnormal cell growth in a mammal which may comprise any one of crystalline salt Forms as described herein, or a pharmaceutical composition thereof, and an amount of one or more substances selected from anti-angiogenesis agents, signal transduction inhibitors, and antiproliferative agents.
  • Anti-angiogenesis agents such as MMP-2 (matrix-metalloprotienase 2) inhibitors, MMP-9 (matrix-metalloprotienase 9) inhibitors, and COX- 11 (cyclooxygenase 11) inhibitors, can be used in conjunction with a compound of the present invention and pharmaceutical compositions described herein.
  • useful COX-II inhibitors include CELEBREXTM (alecoxib), valdecoxib, and rofecoxib.
  • Examples of useful matrix metalloproteinase inhibitors are described in WO 96/33172 (published October 24,1996), WO 96/27583 (published March 7,1996), European Patent Application No.97304971.1 (filed luly 8,1997), European Patent Application No.
  • MMP-2 and MMP-9 inhibitors have little or no activity inhibiting MMP-1, while some selectively inhibit MMP-2 and/or AMP-9 relative to the other matrix-metalloproteinases (L e., MAP-1, NEMP-3, MMP-4, M7vlP-5, MMP-6, MMP- 7, MMP-8, MMP-10, MMP-11, and MMP-13).
  • MlvlP inhibitors useful in the present invention are AG-3340, RU 32-3555, and RS 13-0830.
  • any one of the crystalline salt Forms as described herein, or a pharmaceutical composition thereof, is administered with at least one additional therapeutic agent.
  • the therapeutic agent is a taxol, bortezornib or both.
  • the therapeutic agent is selected from cytotoxic agents, anti- angiogenesis agents and antineoplastic agents.
  • the anti- neoplastic agents selected from the group of consisting of alkylating agents, anti-metabolites, epiclophyllotoxims; antineoplastic enzymes, topoisomerase inhibitors, procarbazine, mitoxantrone, platinum coordination complexes, biological response modifiers and growth inhibitors, hormonal/anti-hormonal therapeutic agents, and haematopoietic growth factors.
  • chemotherapeutics are presently known in the art and can be used in combination with any one of the crystalline salt Forms as described herein, or a pharmaceutical composition thereof.
  • the chemotherapeutic is selected from mitotic inhibitors, alkylating agents, anti-metabolites, intercalating antibiotics, growth factor inhibitors, cell cycle inhibitors, enzymes, topoisomerase inhibitors, biological response modifiers, anti-hormones, angiogenesis inhibitors, and anti-androgens.
  • the combination is administered in combination with an additional therapy.
  • the additional therapy is radiation therapy, chemotherapy, surgery or any combination thereof.
  • the combination is administered in combination with at least one additional therapeutic agent.
  • the therapeutic agent is selected from the group of cytotoxic agents, anti-angiogenesis agents and antineoplastic agents.
  • the anti-neoplastic agent is selected from of alkylating agents, anti-metabolites, epidophyllotoxins; antineoplastic enzymes, topoisomerase inhibitors, procarbazines, mitoxantrones, platinum coordination complexes, biological response 56 ME1 ⁇ 53438692.v1 136867-00920 modifiers and growth inhibitors, hormonal/anti-hormonal therapeutic agents, and haematopoietic growth factors.
  • the second therapeutic is an agent for co-regulating MEK or RAF pathways.
  • the second therapeutic agent is a MEK or RAF inhibitor.
  • the RAF inhibitor is vemurafenib, dabrafenlb, XL-281, LGX-818, CEP-32496.
  • the second therapeutic is an agent for co-regulating MAPK pathway.
  • the agent for co-regulating MAPK pathway is KRAS G12C mutant selective inhibitors including but not limited to sotorasib, adagrasib, ARS-1620, ARS- 3248, LY3499446, AMG-510, and MRTX849; KRAS G12D mutant selective inhibitors; Son of Sevenless 1 (SOS1) inhibitors (e.g., BI1701963, BI-3406 and RMC-023); SHP2 inhibitors (e.g, TNO155, BBP-398 and ICP-189) ; EGFR inhibitors including but not limited to gefitinib, erlotinib, afatinib, lazertinib, aumolertinib (formerly almonertinib), olmutinib, dacomitinib, fasciartinib and osimertinib.
  • KRAS G12C mutant selective inhibitors including but not limited to sotorasib, adagrasib,
  • the second therapeutic is an agent for mutant p53 reactivators (PC14586, APR-246 and COTI-2).
  • the second therapeutic agent is selected from aspirin; diflunisal; salsalate; acetaminophen; ibuprofen; dexibuprofen; naproxen; fenoprofen; ketoprofen; dexketoprofen; flurbiprofen; oxaprozin; loxoprofen; indomethacin; tolmetin; sulindac; etodolac; ketorolac; diclofenac; aceclofenac; nabumetone; enolic acid; piroxicam; meloxicam; tenoxicam; droxicam; lomoxicam; isoxicam; mefenamic acid; meclofenamic acid; flufenamic acid; tolfenamic acid; sulfonanilides; clo
  • the second therapeutic agent is selected from mechlorethamine; cyclophosphamide; melphalan; chlorambucil; ifosfamide; busulfan; N- nitroso-N-methylurea (MNU); carmustine (BCNU); lomustine (CCNU); semustine (MeCCNU); fotemustine; streptozotocin; dacarbazine; mitozolomide; temozolomide; thiotepa; mytomycin; diaziquone (AZQ); cisplatin; carboplatin; and oxaliplatin.
  • MNU N- nitroso-N-methylurea
  • BCNU carmustine
  • CCNU lomustine
  • Semustine MeCCNU
  • fotemustine streptozotocin
  • dacarbazine mitozolomide
  • temozolomide temozolomide
  • thiotepa mytomycin
  • the second therapeutic agent is selected from vincristine; vinblastine; vinorelbine; vindesine; vinflunine; paclitaxel; docetaxel; etoposide; teniposide; tofacitinib; ixabepilone; irinotecan; topotecan; camptothecin; doxorubicin; mitoxantrone; and teniposide.
  • the second therapeutic agent is selected from actinomycin; bleomycin; plicamycin; mitomycin; daunombicin; epimbicin; idarubicin; pirarubicin; aclarubicin; mitoxantrone; cyclophosphamide; methotrexate; 5-fluorouracil; prednisolone; folinic acid; methotrexate; melphalan; capecitabine; mechlorethamine; uramustine; melphalan; chlorambucil; ifosfamide; bendamustine; 6-mercaptopurine; and procarbazine.
  • the second therapeutic agent is selected from cladribine; pemetrexed; fludarabine; gemcitabine; hydroxyurea; nelarabine; cladribine; clofarabine; ytarabine; decitabine; cytarabine; cytarabine liposomal; pralatrexate; floxuridine; fludarabine; colchicine; thioguanine; cabazitaxel; larotaxel; ortataxel; tesetaxel; aminopterin; pemetrexed; pralatrexate; raltitrexed; pemetrexed; carmofur; and floxuridine.
  • the second therapeutic agent is selected from azacitidine; decitabine; hydroxycarbamide; topotecan; irinotecan; belotecan; teniposide; aclarubicin; epimbicin; idarubicin; amrubicin; pirarubicin; valrubicin; zombicin; mitoxantrone; pixantrone; mechlorethamine; chlorambucil; prednimu stine; uramustine; estramustine; carmustine; lomustine; fotemustine; nimustine; ranimustine; carboquone; thioTEPA; triaziquone; and triethylenemelamine.
  • the second therapeutic agent is selected from nedaplatin; satraplatin; procarbazine; dacarbazine; temozolomide; altretamine; mitobronitol; pipobroman; actinomycin; bleomycin; plicamycin; aminolevulinic acid; methyl aminolevulinate; efaproxiral; talaporfin; temoporfin; verteporfin; alvocidib; seliciclib; palbociclib; bortezomib; carfilzomib; anagrelide; masoprocol; olaparib; belinostat; panobinostat; romidepsin; vorinosta; idelalisib; atrasentan; bexarotene; testolactone; amsacrine; trabectedin; alitretinoin; tretinoin; demecolcine; els
  • the second therapeutic agent is selected from azathioprine; Mycophenolic acid; leflunomide; teriflunomide; tacrolimus; cyclosporin; pimecrolimus; abetimus; gusperimus; lenalidomide; pomalidomide; thalidomide; anakinra; sirolimus; everolimus; ridaforolimus; temsirolimus; umirolimus; zotarolimus; eculizumab; adalimumab; afelimomab; certolizumab pegol; golimumab; infliximab; nerelimomab; mepolizumab; omalizumab; faralimomab; elsilimomab; lebrikizumab; ustekinumab; etanercept; otelixizumab; teplizumab; visilizumab;
  • any one of the crystalline salt Forms as described herein, and the additional anti-cancer agent can be administered sequentially, as separate compositions, within an appropriate time frame (e.g., a cancer treatment session/interval (e.g., about 1.5 to about 5 hours to about 10 hours to about 15 hours to about 20 hours; about 1 day to about 2 days to about 5 days to about 10 days to about 14 days)) as determined by the skilled clinician (e.g., a time sufficient to allow an overlap of the pharmaceutical effects of the therapies).
  • a cancer treatment session/interval e.g., about 1.5 to about 5 hours to about 10 hours to about 15 hours to about 20 hours; about 1 day to about 2 days to about 5 days to about 10 days to about 14 days
  • Any one of the crystalline salt Forms as described herein and the additional anti-cancer agent can be administered in a single dose or multiple doses in an order and on a schedule suitable to achieve a desired therapeutic effect (e.g., inhibition of tumor growth).
  • an “effective amount” of any additional therapeutic agent(s) will depend on the type of drug used. Suitable dosages are known for approved therapeutic agents and can be adjusted by the skilled artisan according to the condition of the subject, the type of condition(s) being treated and the amount of a compound of the invention being used by following, for example, dosages reported in the literature and recommended in the Physician’s Desk Reference (57th Ed., 2003).
  • administer means an amount when administered to the subject which results in beneficial or desired results, including clinical results, e.g., inhibits, suppresses or reduces the symptoms of the condition being treated in the subject as compared to a control.
  • a therapeutically effective amount can be given in unit dosage form (e.g., 0.1 mg to about 50 g per day).
  • administered refers to methods that may be used to enable delivery of compositions to the desired site of biological action.
  • Treatment can involve daily or multi-daily or less than daily (such as weekly or monthly etc.) doses over a period of a few days to months, or even years.
  • a person of ordinary skill in the art would immediately recognize appropriate and/or equivalent doses looking at dosages of approved compositions for treating a disease using the disclosed MEK inhibitors for guidance.
  • Any one of the crystalline salt Forms as described herein, or a pharmaceutical composition thereof can be administered to a patient in a variety of forms depending on the selected route of administration, as will be understood by those skilled in the art.
  • the compounds of the present teachings may be administered, for example, by oral, parenteral, buccal, sublingual, nasal, rectal, patch, pump or transdermal administration and the pharmaceutical compositions formulated accordingly.
  • a compound of the present teachings may be incorporated with excipient and used in the form of ingestible tablets, buccal tablets, troches, capsules, elixirs, suspensions, syrups, wafers, and the like.
  • solutions of a compound of the present teachings can generally be prepared in water suitably mixed with a surfactant such as hydroxypropylcellulose.
  • Dispersions can also be prepared in glycerol, liquid polyethylene glycols, DMSO and mixtures thereof with or without alcohol, and in oils. Under ordinary conditions of storage and use, these preparations contain a preservative to prevent the growth of microorganisms.
  • FIG. 34A An XRPD of Form I is shown in Figure 34A and TGA/DSC curves of the starting material are shown in Figure 34B.
  • Table 1 Parameters for XRPD test Model Reflection mode VT-XRPD X-Ray wavelength Cu, k ⁇ , K ⁇ 1 ( ⁇ ): 1.540598, K ⁇ 2 ( ⁇ ): 1.544426 K ⁇ 2/K ⁇ 1 ratio: 0.50 X-Ray tube setting 45 kV, 40 mA 45 kV, 40 mA Divergence slit 1/8o 1/8o Scan mode Continuous Continuous Scan range (°2TH) 3 ⁇ 40 3 ⁇ 40 Scan step time (s) 46.67 33.02 Step size (°2TH) 0.0263 0.0167 Test time approximately 5 min 4 s Approximately 10 min 17 s TGA and DSC TGA data were collected using a Discovery TGA 5500/TGA 550 TGA from TA Instruments and DSC was performed using a Discovery DSC 2500/DSC 250 DSC from TA 64 ME1 ⁇ 53438692.v1 136867-00920 Instruments.
  • Table 2 Parameters for TGA and DSC test Parameters TGA DSC Method Ramp Ramp Sample pan Aluminum, open Aluminum, crimped Temperature RT ⁇ 350 oC 25 °C ⁇ 300 oC Heating rate 10 oC/min 10 oC/min Purge gas N 2 N 2 UPLC A Waters H-Class UPLC with PDA detector was utilized and detailed chromatographic conditions for purity and stoichiometric ratio analysis were listed in Table .
  • XRPD patterns of the re-prepared salt samples were consistent with XRPD patterns of reference materials (see Figures 35A, 36A, 37A, 38A, and 39A).
  • DSC and TGA thermograms of the re-prepared salt samples are shown in Figures 35B, 36B, 37B, 38B, and 39B.
  • 70 ME1 ⁇ 53438692.v1 136867-00920 Polymorph Screening of Certain Salts The re-prepared salt samples described above were used for polymorph screening experiments. General Methods Slurry at RT/50 oC For each experiment, about 18 mg of the indicated starting material was suspended in 0.5 mL corresponding solvent in an HPLC glass vial.
  • Table 11A Peaks list of K salt Form II 73 ME1 ⁇ 53438692.v1 136867-00920 2 ⁇ [°] Rel [%] 4.4 43.7 7.8 24.4 8.6 42.0 10.8 10.9 12.9 18.4 13.7 19.1 14.4 81.5 17.2 37.7 17.5 100.0 18.4 41.8 18.9 26.2 21.5 44.8 22.8 3.6 23.5 35.4 24.0 54.1 27.6 31.5 28.0 7.7 30.1 16.5 30.4 10.6 31.1 22.3 32.2 9.1 33.9 10.8 36.6 16.5
  • Table 12B UPLC result of K salt Form II # Peak RRT Area% # Peak RRT Area% 1 0.48 0.48 6 1.00 97.68 2 0.51 1.09 7 1.11 0.05 3 0.65 0.14 8 1.43 0.10 4 0.75 0.05 9 1.44 0.06 5 0.92 0.36 -- -- -- -- 74 ME1 ⁇ 53438692.v1 136867-00920 K Salt Form III K salt Form III was obtained via anti-solvent addition in DMSO/MTBE system at
  • Table 12A Peaks list of K salt Form III 2 ⁇ [°] Rel [%] 7.2 33.5 9.3 25.0 10.2 58.4 10.9 3.1 11.4 4.4 11.8 3.4 12.0 9.2 12.7 5.8 13.2 13.0 13.6 25.4 14.4 4.6 15.0 44.3 17.0 100.0 17.7 10.1 18.1 9.3 20.4 43.1 21.4 4.3 75 ME1 ⁇ 53438692.v1 136867-00920 2 ⁇ [°] Rel [%] 23.9 24.6 37.9 6.9
  • Table 13B UPLC result of K salt Form III # Peak RRT Area% # Peak RRT Area% 1 0.48 0.53 4 0.92 0.19 2 0.51 0.89 5 1.00 98.32 3 0.65 0.07 -- -- -- Na Salt Forms A total of seven forms of sodium salt of Compound 1 were observed from salt/co- crystal and polymorph screening experiments, named as Na salt Forms I-VII.
  • XRPD results of initially prepared batch of Na salt Form II are shown in Error! Reference source not found.. XRPD peaks are listed in Table 15A. UPLC/IC results showed that the molar ratio of Na+/freeform was 1.1 and the purity was 98.28 area%. UPLC results are displayed in Table 15B and in Figure 4D. TGA/DSC results of Na salt Form II are shown in Figure 4B. TGA result showed a weight loss of 5.96% up to 180 oC. DSC result showed three endotherms at 65.3, 118.5 and 179.3 oC (peak temperature) NMR result in Figure 4C showed negligible residual solvent ACN.
  • Table 15A Peaks list of Na salt Form II 2 ⁇ [°] Rel [%] 6.5 100.0 7.6 22.5 8.4 12.6 11.5 6.9 14.7 21.0 15.2 28.7 17.1 18.3 77 ME1 ⁇ 53438692.v1 136867-00920 2 ⁇ [°] Rel [%] 18.0 18.7 18.9 4.8 19.5 6.6 20.9 6.0 22.9 87.6
  • Table 15B UPLC result of Na salt Form # Peak RRT Area% # Peak 1 0.48 0.49 5 1.00 98.28 2 0.52 0.64 6 1.44 0.10 3 0.65 0.10 7 1.52 0.05 4 0.91 0.32 -- -- Na Salt Form III After slurrying of Compound 1 and equal molar NaOH in acetone at RT for 7 days and at 5 oC for 3 days, followed by the addition of anti-solvent MTBE, slurrying at RT for 5 days and drying at RT under vacuum for approximately 6 hrs, Na salt Form III was obtained.
  • XRPD result is shown in Figure 5A.
  • XRPD peaks are listed in Table 16A.
  • UPLC/IC results show that the molar ratio of Na+/freeform was 1.1 and the purity was 98.95 area%.
  • UPLC results are displayed in Table 16B and in Figure 5D.
  • TGA/DSC results are shown in Figure 5B.
  • TGA result shows a weight loss of 0.97% up to 140 oC and 17.04% between 140 oC and 280 oC.
  • DSC result shows an endotherm at 179.8 oC (peak temperature)
  • NMR result in Figure 5C reveals that the molar ratio of residual solvent DMSO/API was 1.4 (17.5 wt%, close to the second step weight loss).
  • XRPD results are shown in Figure 7A. XRPD peaks are listed in Table 18A. UPLC/IC results showed that the molar ratio of Na+/freeform was 1.0 and the purity was 99.61 area%. UPLC results are displayed in Table 18B and in Figure 7D. TGA/DSC results are shown in Figure 7B. TGA showed a weight loss of 2.92% up to 120 oC and 14.99% between 120 oC and 250 oC. DSC result showed two endotherms at 112.0 and 134.8 oC (peak temperature) NMR result in Figure 7C revealed that the molar ratio of residual solvent NMP/API was 0.9 (14.8 wt%, close to the second step weight loss).
  • VT-XRPD was performed on Na salt Form V and the results are shown in Figure 7E.
  • a form change was observed after N 2 purging for 20 min at 25 oC. No further form change was observed after heating to 112 oC and cooling to 25 oC with N2 protection. After exposure to ambient conditions for 30 min, Na salt Form V was re- obtained. Based on the results, Na salt Form V was speculated to be a hydrate. In addition, after heating Na salt Form V to 200 oC and cooling to RT to remove the solvent NMP, the sample melted, suggesting that Na salt Form V also may be a NMP solvate. Based on the characterization results, Na salt Form V was proposed to be a water-NMP co-solvate. NMP may be removed after the sample melted.
  • Table 18A Peaks list of Form V 2 ⁇ [°] Rel [%] 8.6 8.7 9.3 17.1 9.6 51.5 10.8 35.7 11.2 9.0 11.6 6.0 12.9 5.5 13.4 4.1 13.6 5.6 14.6 23.6 15.5 10.6 16.2 94.6 16.9 26.4 81 ME1 ⁇ 53438692.v1 136867-00920 2 ⁇ [°] Rel [%] 17.2 21.4 17.5 50.3 17.9 32.6 18.4 29.9 18.8 16.7 19.0 30.0 19.7 100.0 20.9 10.6 22.1 35.6 22.8 16.5 23.3 43.3 23.5 25.2 24.3 37.7 28.4 6.0 28.7 9.7 29.5 21.3 31.3 8.3 32.7 8.6 33.8 0.5 Table 18B: UPLC result of Na salt Form V # Peak RRT Area% # Peak RRT Area% 1 0.48 0.19 3 1.00 99.61 2 0.51 0.12 4 1.49 0.08 Na Salt Form VI Na salt Form VI was obtained via slurry of Na salt Form II in DMAc/H 2 O (1:
  • XRPD results are shown in Figure 8A. XRPD peaks are listed in Table 19A. UPLC/IC results showed that the molar ratio of Na+/freeform was 1.0 and the purity was 99.36 area%. UPLC results are displayed in Table 19B and in Figure 8D. TGA/DSC results are shown in Figure 8B. TGA result showed a stepwise weight loss of 13.48% up to 170 oC. DSC result showed 82 ME1 ⁇ 53438692.v1 136867-00920 four endotherms at 49.9, 100.2, 116.9 and 154.6 oC (peak temperature).
  • Table 19A Peaks list of Na salt Form VI 2 ⁇ [°] Rel [%] 6.4 23.8 10.6 100.0 10.9 6.7 11.6 13.0 11.8 7.9 12.9 37.4 13.1 18.4 14.4 99.7 15.2 27.5 16.2 52.1 17.2 23.0 18.3 44.0 19.3 47.7 19.6 71.0 20.4 21.8 21.4 22.5 22.5 13.9 22.9 60.0 23.3 47.9 24.5 12.8 29.0 24.9 30.7 18.5 83 ME1 ⁇ 53438692.v1 136867-00920 2 ⁇ [°] Rel [%] 32.8 8.6 38.0 9.7 Table 19B: UPLC result of Na salt Form VI # Peak RRT Area% # Peak RRT Area% 1 0.48 0.14 3 1.00 99.36 2 0.51 0.50 -- -- -- -- Na salt Form VII Na salt Form VII was obtained via slurry of Na salt Form II in acetone at RT for 7 days, followed by air-drying at RT.
  • XRPD result is shown in Error! Reference source not found.
  • XRPD peaks are listed in Table 20A.
  • UPLC/IC results showed that the molar ratio of Na + /freeform was 1.0 and the purity was 98.67 area%.
  • UPLC results are displayed in Table and in Error! Reference source not found.
  • TGA/DSC results are shown in Error! Reference source not found..
  • TGA result showed a weight loss of 0.89% up to 110 oC and 6.47% between 110 oC and 170 oC.
  • DSC result showed two endotherms at 154.7 and 184.2 oC (peak temperature) NMR result in Error! Reference source not found.
  • Table 20A Peaks list of Na salt Form VII 2 ⁇ [°] Rel [%] 9.6 100.0 9.9 48.4 12.9 30.1 15.0 6.5 15.5 84.7 16.4 14.0 17.2 75.5 84 ME1 ⁇ 53438692.v1 136867-00920 2 ⁇ [°] Rel [%] 18.1 71.7 19.2 39.5 19.8 31.3 21.1 16.4 21.2 17.3 21.5 31.0 22.3 48.6 23.2 87.9 29.0 45.7 30.0 7.7 31.1 20.3 32.0 20.8 34.5 17.8 35.3 15.5
  • Table 20B UPLC result of Na salt Form VII # Peak RRT Area% # Peak RRT Area% 1 0.48 0.47 4 0.92 0.12 2 0.51 0.64 5 1.00 98.67 3 0.68 0.06 6 1.42 0.05 Ca Salt Forms A total of five forms of calcium salt of Compound 1 were observed from polymorph screening experiments, named as Ca salt Forms I-V.
  • XRPD patterns are displayed in Figures 10A, 11A, 12A, 13A, and 14.
  • the XPRD overlay pattern of Ca salt Forms I-V is displayed in Figure 10F. Additional characterization results are summarized in Table 21.
  • Table 21 Characterization summary of Ca salt forms Crystal form Weight loss in DSC Molar Solvent UPLC endother Speculated TGA (%) m ratio residue purity form Ca salt Form III 0.66 (150 oC) 216.0 0.5 17.8 98.81 DMSO 85 ME1 ⁇ 53438692.v1 136867-00920 Crystal form Weight loss in DSC Molar Solvent UPLC TGA (%) endotherm Speculated ratio residue purity (oC, peak) (Ca2+/API) (wt%) (area%) form 7.51 (150-210 oC) (DMSO) solvate Ca salt Form V Data not collected.
  • Ca Salt Form I was generated as follows: 1) slurry of Compound 1 free Form I and equal molar Ca(OH) 2 in acetone at RT for 9 days, 2) additional Compound 1 free Form I was added (the charge ratio of total freeform/Ca(OH)2 was 2:1) and slurry at RT for 5 days, 3) air- dry the sample at RT for 4 hrs, XRPD pattern is shown in Error! Reference source not found.. XRPD peaks are listed in Table 22A. UPLC/IC results confirmed that the molar ratio of Ca 2+ /freeform was 0.4 and the purity was 96.88 area%. UPLC results are displayed in Table and in Error! Reference source not found..
  • TGA/DSC results are shown in Error! Reference source not found.
  • TGA result showed a weight loss of 7.11% up to 180 oC.
  • DSC result showed three endotherms at 73.1, 135.8 and 200.2 oC (peak temperature) NMR result in Error! Reference source not found. showed that the molar ratio of residual solvent acetone/API was 0.02 (0.2 wt%).
  • VT-XRPD was performed for form identification and the results are displayed in Error! Reference source not found..
  • Form change was observed after N2 purging Ca salt Form I with N2 for 20 min at 25 oC. After heating to 80 oC, 150 oC and cooling to 25 oC with N2 protection, further form change was observed.
  • Peak shift at 200 oC may be caused by the expansion of the crystal lattice at high temperature.
  • Table 23A Peaks list of Ca salt Form II 2 ⁇ [°] Rel [%] 4.3 100.0 7.0 6.2 8.3 67.1 8.6 25.2 10.0 6.7 10.8 19.4 12.2 5.7 13.0 21.2 14.0 69.9 14.9 17.1 15.9 22.0 17.3 23.5 18.0 5.6 18.4 10.9 20.2 8.3 23.2 19.0
  • Table 23B UPLC result of Ca salt Form II # Peak RRT Area% 1 0.48 0.54 2 0.52 0.56 3 0.91 0.07 88 ME1 ⁇ 53438692.v1 136867-00920 4 1.00 98.83
  • Ca Salt Form III Ca salt Form III was obtained via the following procedure: 1) slurry Compound 1 free Form I and equal molar Ca(OH) 2 in DMSO/EtOH (1:3, v/v) at RT for 9 days, 2) additional Compound 1 free Form I was added (the charge ratio of extra freeform/Ca
  • XRPD pattern is shown in Figure 12A.
  • XRPD peaks are listed in Table 24A.
  • UPLC/IC results confirmed that the molar ratio of Ca 2+ /freeform was 0.5 and the purity was 98.81 area%.
  • the UPLC results are displayed in Table 24B and in Error! Reference source not found..
  • TGA/DSC results are shown in Figure 12B.
  • TGA showed a three-step weight loss of 0.86% (to 150 oC), 7.51% (150-210 oC) and 11.36% (210-260 oC).
  • DSC showed an endotherm at 216.0 oC (peak temperature)
  • NMR result in Figure 12C showed that the molar ratio of residual solvent DMSO/API was 1.4 (17.8 wt%).
  • Table 24A Peaks list of Ca salt Form III 2 ⁇ [°] Rel [%] 9.2 15.4 11.0 18.4 12.6 29.7 13.3 20.0 14.0 89.8 15.4 45.2 15.9 7.1 16.4 16.2 17.3 37.1 18.1 10.6 18.7 100.0 19.3 33.5 20.0 34.1 20.5 27.6 89 ME1 ⁇ 53438692.v1 136867-00920 2 ⁇ [°] Rel [%] 21.2 19.4 22.0 18.1 22.8 55.0 24.0 20.9 30.3 7.8 31.1 9.4 31.4 17.6 32.7 10.6 33.5 16.7 34.2 6.4 34.7 9.2 36.8 11.2
  • Table 24B UPLC result of Ca salt Form III # Peak RRT Area% 1 0.48 0.18 2 0.52 0.83 3 0.91 0.11 4 1.00 98.81 5 1.43 0.07 Ca Salt Form IV/V Ca salt Form IV was obtained via the following procedure: after slurry of Ca salt Form II in MeOH/DCM (1:1, v/v) at RT for 7 days, clear solution
  • Ca salt Form V is proposed to be a hydrate.
  • Table 25A Peaks list of Ca salt Form IV 2 ⁇ [°] Rel [%] 6.6 92.5 7.4 63.7 8.4 31.7 11.2 32.7 12.6 34.3 13.1 19.2 13.6 20.2 14.4 16.5 14.8 34.4 15.9 12.6 16.8 22.5 17.5 82.5 18.2 18.5 21.1 25.9 22.2 100.0 23.3 33.2 35.2 11.1 91 ME1 ⁇ 53438692.v1 136867-00920
  • Table 25B UPLC result of Ca salt Form IV # Peak RRT Area% # Peak RRT Area% 1 0.48 0.51 5 0.89 0.05 2 0.51 1.37 6 1.00 97.63 3 0.53 0.08 7 1.14 0.12 4 0.63 0.06 8 1.18 0.18
  • Table 25C Peaks list of Ca salt Form V 2 ⁇ [°] Rel [%] 6.4 40.6 7.0 34.8 7.7 14.3 8.3 7.9 9.3 10.5 12.5 21.7 13.9 32.0 15.4 16.7 17.5 100.0 20.0 4.4 21.1 10.9 22.2 12.1 23.3 41.5 24.6 1
  • XRPD patterns are displayed in Figures 15A, 16, 17A, 18A, 19A, and 20A.
  • XPRD overlay patterns of Choline salt Forms I- VI are displayed in Figure 15F. Additional characterization results are summarized in Table 26.
  • Table 26 Characterization summary of Choline salt forms Crystal form Weight loss in DSC Molar Solvent UPLC TGA (%) endotherm Speculated ratio residue purity (oC, peak) (base/API) (wt%) (area%) form Choline salt Form I 0.78 (180 oC) 172.1 1.0 0.1 9 9.47 Anhydrate (re-prep batch) Choline salt 13 Form III 2.43 (150 oC) 1.8, 135.3*, 175.7 1.1 1.9 (MeOH) 99.81 Anhydrate Choline salt 116.4, 142.3, EtOH 6.2 F orm IV 7.02 (130 oC) 144.6*, 176.2 (EtOH) solvate Choline salt Form V 2.17 (170 oC) 142.2, 144.8*, 176.3 1.1 Not
  • Choline Salt Form I Initial preparation of Choline salt Form I is described in the Salt Preparations section above. Characterization results are given in Table 7. As also described above (see Table 8), Choline salt Form I was re-prepared. As shown in overlay Figure 38A, the XRPD pattern of the re-prepared salt sample was consistent with that of the initial sample. The re-prepared material was used in further choline salt polymorph screening. XRPD pattern of the re- prepared sample is shown in Error! Reference source not found. XRPD peaks are listed in Table 27A. TGA/DSC results in Figure 15B showed a weight loss of 0.78% up to 180 oC and an endotherm at 172.1 oC (peak temperature).
  • XRPD pattern is shown in Error! Reference source not found. XRPD peaks are listed in Table 28. After drying at RT under vacuum overnight, a form change to Choline salt Form VI was observed (an extra peak marked by the black star was observed, see XRPD overlay in Figure 16B).
  • TGA showed a weight loss of 2.43% up to 150 oC.
  • DSC showed two endotherms at 131.8 and 175.7 oC and an exotherm at 135.3 oC (peak temperature)
  • NMR in Figure 17C revealed that the molar ratio of choline/freeform was 1.1 and the residual solvent MeOH/API was 0.4 (1.9 wt%).
  • UPLC result showed that the purity was 99.81 area%.
  • UPLC results are listed in Table 29B and in Figure 17D. After heating Choline salt Form III to 110 oC and cooling to RT, a mixture of Choline salt Form III+VI was observed (peaks of Choline salt Form VI were observed. Choline salt Form VI was identified to be an anhydrate).
  • Table 29A Peaks list of Choline salt Form III 2 ⁇ [°] Rel [%] 7.4 72.7 11.1 16.3 12.6 1.3 14.8 100.0 16.5 3.8 17.5 0.7 18.3 1.5 18.6 5.6 19.1 0.6 20.3 2.3 21.2 1.9 22.3 20.3 22.9 0.9 31.7 0.8 33.4 2.3 96 ME1 ⁇ 53438692.v1 136867-00920
  • Table 29B UPLC result of Choline salt Form III # Peak RRT Area% 1 0.48 0.19 2 1.00 99.81 Choline Salt Form IV Choline salt Form IV was obtained via slurry of Choline salt Form I in EtOH at 50 oC for 7 days, followed by air-drying at RT for approximately 8.5 hrs.
  • XRPD results are shown in Figure 18A and in Table 30A.
  • TGA/DSC results were shown in Figure 18B.
  • TGA result showed a stepwise weight loss of 7.02% up to 130 oC.
  • DSC result showed three endotherms at 116.4, 142.3 and 176.2 oC and an exotherm at 144.6 oC (peak temperature) result in Figure 18C revealed that the molar ratio of choline/freeform was 1.1 and residual solvent EtOH/API was 0.9 (6.2 wt%, close to the TGA weight loss).
  • UPLC result showed that the purity was 99.94 area%.
  • UPLC results are listed in Table 30B and in Figure 18D.
  • Choline salt Form V After heating Choline salt Form IV to 120 oC and cooling to RT, a new form was obtained, which was named as Choline salt Form V. After heating Choline salt Form IV to 140 oC and cooling to RT, Choline salt Form VI was obtained. The VT-XRPD comparison results were shown in Figure 18E. Based on the characterization and heating results, Choline salt Form IV was proposed to be an EtOH mono-solvate.
  • Table 30A Peaks list of Choline salt Form IV 2 ⁇ [°] Rel [%] 6.7 8.2 10.0 8.8 10.5 79.2 11.3 21.7 11.6 5.8 13.3 30.0 13.9 7.4 15.4 9.1 16.2 5.9 17.4 100.0 17.8 25.3 18.3 87.0 97 ME1 ⁇ 53438692.v1 136867-00920 2 ⁇ [°] Rel [%] 18.9 10.6 20.5 8.6 20.7 30.9 21.1 20.1 22.3 10.1 23.0 7.1 23.4 13.1 23.8 30.0 24.3 11.4 33.1 4.6
  • Table 30B UPLC result of Choline salt Form IV # Peak RRT Area% 1 0.51 0.06 2 1.00 99.94 Choline Salt Form V Choline salt Form V was obtained via heating Choline salt Form IV to 120 oC, cooling to RT and exposure to ambient conditions.
  • XRPD results are shown in Figure 19A and in Table 31A.
  • TGA/DSC results are shown in Figure 19B.
  • TGA result showed a gradual weight loss of 2.17% up to 170 oC.
  • DSC result showed two endotherms at 142.2 and 176.3 oC and an exotherm at 144.8 oC (peak temperature)
  • NMR result in Figure 19C revealed that the molar ratio of choline/freeform was 1.1 and negligible residual solvent was detected.
  • UPLC result showed that the purity was 99.93 area%.
  • UPLC results are listed in Table 31B and in Figure 19D. Based on the characterization results, Choline salt Form V may be an anhydrate.
  • Table 4 Peaks list of Choline salt Form V 2 ⁇ [°] Rel [%] 7.3 11.2 10.6 89.8 10.9 9.4 98 ME1 ⁇ 53438692.v1 136867-00920 2 ⁇ [°] Rel [%] 11.4 27.9 14.5 41.0 15.0 5.8 15.6 20.1 16.2 11.7 16.9 11.4 17.4 100.0 17.8 23.3 18.6 86.4 19.8 26.0 20.7 42.3 21.2 41.3 22.0 7.5 23.3 13.5 24.2 23.3
  • Table 31B UPLC result of Choline salt Form V # Peak RRT Area% 1 0.51 0.07 2 1.00 99.93 Choline Salt Form VI Choline salt Form VI was obtained via drying Choline salt Form II under vacuum at RT overnight.
  • XRPD results are shown in Figure 20A and Table 32A.
  • TGA/DSC results are shown in Figure 20B.
  • TGA showed a gradual weight loss of 1.27% up to 170 oC.
  • DSC showed an endotherm at 174.6 NMR result in Figure 20C revealed that the molar ratio of choline/freeform was 1.1 and residual solvent DMSO/API was 0.09 (1.1 wt%).
  • UPLC result showed that the purity was 99.46 area%.
  • UPLC results are displayed in Table 32B and in Figure 20D. Based on the characterization results, Choline salt Form VI is proposed to be an anhydrate.
  • Table 32A Peaks list of Choline salt Form VI 99 ME1 ⁇ 53438692.v1 136867-00920 2 ⁇ [°] Rel [%] 9.5 7.9 11.2 50.9 11.4 13.7 12.9 15.3 14.1 24.7 14.4 29.6 15.3 6.2 16.1 30.1 16.4 100.0 16.7 23.2 17.0 41.7 17.8 9.9 18.1 6.0 18.9 27.8 19.3 36.4 19.7 14.4 20.0 39.7 20.4 64.3 21.1 26.7 22.1 12.5 22.4 31.2 22.9 49.2 23.4 11.4 23.7 8.9 28.3 6.6 33.2 7.9
  • Table 32B UPLC result of Choline salt Form VI 100 ME1 ⁇ 53438692.v1 136867-00920 # Peak RRT Area% 1 0.49 0.09 2 0.51 0.39 3 0.92 0.05 4 1.00 99.46 Hydrogen Bromide (HBr) Salt Forms A total of three forms of HBr salt of Compound 1 were observed from polymorph screening experiments, named as HBr salt Forms I, II and III
  • XRPD patterns are displayed in Figures 21A, 22A, and 23.
  • the XPRD overlay pattern of HBr salt Forms I-III is displayed in Figure 21E. Additional characterization results are summarized in Table 33.
  • Table 33 Characterization summary of HBr salt forms m Weight loss in DSC Molar Solvent UPLC Crystal for Speculated TGA (%) endotherm ratio residue purity form determined *: Peaks of Compound 1 Form I were also observed, suggesting that the sample may be a mixture HBr salt (a new form) and freeform.
  • HBr Salt Form I HBr salt Form I was obtained via slurry of Compound 1 free Form I and equal molar HBr in acetone at RT for 4 days and air-drying at RT overnight.
  • XRPD results are shown in Figure 21A and Table 34A.
  • TGA/DSC results are shown in Figure 21B.
  • TGA showed a weight loss of 9.40% up to 160 oC.
  • DSC showed four endotherms at 81.9, 116.7, 146.8 and 169.7 oC (peak temperature).
  • 1 H NMR result showed that the molar ratio of residual solvent acetone/API was 0.02 (0.2 wt%).
  • UPLC/IC results showed that the purity was 98.01 area% and the stoichiometric ratio of Br-/freeform was only 0.7.
  • UPLC results are displayed in Table 34B and in Figure 21D.
  • Table 34A Peaks list of HBr salt Form I 2 ⁇ [°] Rel [%] 4.8 37.8 8.7 29.7 101 ME1 ⁇ 53438692.v1 136867-00920 2 ⁇ [°] Rel [%] 9.6 17.5 12.4 11.4 13.2 25.5 14.5 24.9 14.9 25.8 15.2 41.8 15.8 26.3 16.9 12.1 17.5 16.8 17.7 100.0 19.4 15.5 21.1 15.2 22.8 10.7 24.1 32.7 30.0 46.0
  • Table 34B UPLC result of HBr salt Form I # Peak RRT Area% 1 0.52 1.93 2 1.00 98.01 3 1.43 0.07 HBr Salt Form II Initial preparation of HBr salt Form II is described in the Salt Preparations section above.
  • HBr salt Form II After exposure to ambient conditions, HBr salt Form II (with two additional peaks (highlighted by red stars) consistent with the sample after cooling to 25 oC was re- obtained, indicating that HBr salt Form II was a hydrate (the theoretical water content of monohydrate was 3.0 wt%).
  • Table 35A Peaks list of HBr salt Form II 2 ⁇ [°] Rel [%] 4.9 58.1 6.8 11.8 9.7 19.5 10.8 33.9 12.8 5.5 13.7 7.1 14.5 35.1 15.3 100.0 15.6 24.5 16.3 7.7 17.4 14.3 19.4 26.3 20.5 8.5 21.6 12.1 22.9 4.9 23.6 27.5 24.2 29.8 28.6 5.0 29.2 12.5 29.7 4.7 30.8 12.8 103 ME1 ⁇ 53438692.v1 136867-00920 2 ⁇ [°] Rel [%] 31.7 5.8 34.2 4.2 35.3 4.0
  • Table 35B UPLC result of HBr salt Form II # Peak RRT Area% 1 0.52 1.06 2 0.65 0.05 3 0.92 0.08 4 1.00 98.82 HBr Salt Form III HBr salt Form III was obtained via adding anti-solvent n-heptane into THF solution of HBr salt Form II.
  • NMR result showed that the molar ratio of residual solvent acetone/API was 0.07 (0.6 wt%) and the stoichiometric ratio of acid/freeform was 0.7.
  • UPLC results confirmed that the purity was 93.39 area%.
  • Table 37A Peaks list of 1,5-Naphthalenedisulfonate Form I 2 ⁇ [°] Rel [%] 7.5 22.9 8.3 36.5 10.6 18.3 11.1 58.0 11.8 18.5 12.2 32.8 12.4 16.2 13.1 23.3 13.7 13.7 14.0 42.6 105 ME1 ⁇ 53438692.v1 136867-00920 2 ⁇ [°] Rel [%] 14.5 22.2 15.0 24.1 15.7 72.5 16.0 33.6 16.4 23.3 16.7 26.4 16.9 25.4
  • Table 37B UPLC result of 1,5-Naphthalenedisulfonate Form I # Peak RRT Area% 1 0.52 6.31 2 0.65 0.13 3 0.91 0.07 4 1.00 93.39 5 1.44 0.11 1,5-Naphthalenedisulfonate Salt Form II 1,5-Naphthalenedisulfonate Form II was obtained via slurry of Compound 1 free Form I and equal molar 1,5-naphthalenedisulfonic acid in ACN at RT for 3 days and drying at RT under vacuum
  • XRPD results are shown in Figure 25A and Table 38A.
  • TGA/DSC curves are shown in Figure 25B.
  • TGA showed a weight loss of 5.48% up to 150 oC.
  • DSC showed three endotherms at 130.9 oC, 155.2 oC and 164.3 oC and one exotherm at 143.7 oC (peak temperature).
  • NMR result showed that residual solvent ACN/API was 0.08 (0.7 wt%) and the stoichiometric ratio of acid/freeform was 0.9.
  • UPLC results confirmed that the purity was 90.82 area%.
  • Table 38A Peaks list of 1,5-Naphthalenedisulfonate Form II 2 ⁇ [°] Rel [%] 5.9 15.6 7.5 7.2 8.3 3.6 11.1 3.6 106 ME1 ⁇ 53438692.v1 136867-00920 2 ⁇ [°] Rel [%] 12.9 3.1 13.2 22.9 14.1 11.7 14.5 6.3 15.0 6.5 15.7 14.2 18.2 20.5 18.6 15.1 19.9 4.8 22.1 1.9 22.5 7.4 23.2 16.6 25.8 95.9 26.3 100.0 31.4 2.8 32.8 3.0
  • Table 38B UPLC result of 1,5-Naphthalenedisulfonate Form II # Peak RRT Area% 1 0.51 8.83 2 0.64 0.10 3 0.91 0.14 4 1.00 90.82 5 1.44 0.10 1,2-Ethanedisulfonic (Edisylate) Salt Forms 107 ME1 ⁇ 53438692.v1 136867-00920 A total of two forms of Edisylate, named as Edisylate Form I and Ed
  • XRPD results are shown in Figure 27A and Table 40A.
  • TGA/DSC curves were shown in Figure 27B.
  • TGA showed a weight loss of 3.71% up to 160 oC.
  • DSC showed three endotherms at three endotherms at 74.2, 116.5 and 131.1 oC (peak temperature).
  • NMR result showed that negligible solvent ACN was detected and the stoichiometric ratio of acid/freeform was 0.8.
  • UPLC results confirmed that the purity was 92.77 area%.
  • Table 40A Peaks list of Edisylate Form II 2 ⁇ [°] Rel [%] 6.0 100.0 10.8 8.6 13.5 13.1 16.6 51.3 17.2 31.2 17.5 17.7 18.2 21.2 19.1 11.1 21.3 34.1 21.7 19.6 22.4 18.2 23.0 16.6
  • Table 40B UPLC result of Edisylate Form II # Peak RRT Area% 1 0.52 6.97 2 0.64 0.07 3 0.91 0.05 4 1.00 92.77 5 1.09 0.07 6 1.44 0.07 Diethylamine Salt Forms 109 ME1 ⁇ 53438692.v1 136867-00920 A total of two forms of Diethylamine salt, named as Diethylamine salt Form I and Diethylamine salt Form II, were obtained from salt screening experiments.
  • Diethylamine Salt Form I Diethylamine salt Form I was obtained via slurry of Compound 1 free Form I and equal molar diethylamine in ACN at RT for 4 days. XRPD results are shown in Figure 28A and Table 41A. TGA/DSC curves are shown in Figure 28B. TGA showed a weight loss of 7.30% up to 100 oC. DSC showed two endotherms at 98.7 oC and 195.9 oC (peak temperature).
  • NMR result showed that the molar ratio of residual solvent ACN/API was 0.4 (3.0 wt%) and the stoichiometric ratio of diethylamine/freeform was 0.5.
  • UPLC results confirmed that the purity was 99.22 area%.
  • Figure 28E after Diethylamine salt Form I was heated to 110 oC, followed by being cooled down to RT and exposure to ambient conditions, Compound 1 free Form I was observed, suggesting that the TGA weight loss may be caused by the loss of diethylamine.
  • Table 41A Peaks list of Diethylamine salt Form I 2 ⁇ [°] Rel [%] 8.7 16.2 9.2 5.4 12.9 22.4 13.2 13.3 13.4 26.2 14.9 15.3 15.1 14.4 15.8 11.1 16.8 9.2 17.0 11.1 17.7 100.0 18.6 5.2 19.0 23.6 19.5 7.2 20.1 8.5 20.3 11.2 110 ME1 ⁇ 53438692.v1 136867-00920 2 ⁇ [°] Rel [%] 20.9 5.1 21.1 10.4 21.4 21.8 23.4 10.2 24.3 8.7 25.0 45.3 29.3 5.3 30.0 19.9 30.9 4.3 32.2 3.1
  • Table 41B UPLC result of Diethylamine salt Form I # Peak RRT Area% 1 0.48 0.21 2 0.52 0.43 3 0.92 0.14 4 1.00 99.22 Diethylamine Salt Form II Diethylamine salt Form II was obtained via procedure as follows: 1) Slurry of Compound 1 free Form I and equal molar diethylamine in acetone at RT for 9
  • XRPD results are shown in Figure 29A and Table 42A.
  • TGA/DSC curves are shown in Figure 29B.
  • TGA showed a weight loss of 18.31% up to 160 oC.
  • DSC showed three endotherms at 119.8, 180.0 and 192.0 oC (peak temperature).
  • NMR result showed that the molar ratio of residual solvent acetone/API was 0.2 (1.9 wt%) and the stoichiometric ratio of diethylamine/freeform was 0.9.
  • UPLC results confirmed that the purity was 99.62 area%.
  • Table 42A Peaks list of Diethylamine salt Form II 111 ME1 ⁇ 53438692.v1 136867-00920 2 ⁇ [°] Rel [%] 3.7 15.4 7.3 18.1 8.5 4.5 10.3 6.7 11.0 100.0 12.3 15.7 13.8 18.6 14.6 42.8 16.9 23.7 17.9 36.2 18.2 12.2 20.9 4.3 22.9 7.0 23.5 3.6
  • Table 42B UPLC result of Diethylamine salt Form II # Peak RRT Area% 1 0.48 0.09 2 0.52 0.24 3 0.92 0.05 4 1.00 99.62 Hydrogen Chloride (HCl) Salt Forms A total of four forms of HCl salt of Compound 1 was obtained. Initial salt screening provided HCl salt Forms I, II and III.
  • HCl Salt Form I HCl salt Form I was prepared via slurry of Compound 1 free Form I and equal molar HCl in ACN at RT for 4 days and air-drying at RT overnight. XRPD results are shown in Figure 30A and Table 43A. TGA/DSC curves are shown in Figure 30B. TGA showed a weight loss of 7.65% up to 150 oC. DSC showed four endotherms at 93.9, 137.6, 153.4 and 112 ME1 ⁇ 53438692.v1 136867-00920 166.7 oC (peak temperature).
  • Table 43A Peaks list of HCl salt Form I 2 ⁇ [°] Rel [%] 4.8 89.3 6.8 24.2 9.7 19.5 10.7 9.3 12.3 4.1 13.5 5.8 14.4 20.2 15.3 100.0 15.9 19.5 17.3 6.3 19.4 24.4 21.7 10.2 24.1 34.4 29.2 19.6 30.9 12.2
  • Table 43B UPLC result of HCl salt Form I # Peak RRT Area% 1 0.52 1.54 2 1.00 98.34 3 1.38 0.05 4 1.43 0.07 HCl Salt Form II HCl salt Form II was obtained via slurry of Compound 1 free Form I and equal molar HCl in acetone at RT for 3 days. XRPD results are shown in Figure 31 and Table 44.
  • Table 45 Peaks list of HCl salt Form III 114 ME1 ⁇ 53438692.v1 136867-00920 2 ⁇ [°] Rel [%] 4.8 97.6 6.3 63.9 8.1 43.1 8.7 61.0 9.6 26.5 10.8 6.7 13.3 17.5 14.2 77.4 15.8 22.9 16.5 92.1 17.4 26.4 17.8 15.1 19.2 47.4 19.5 16.2 20.3 38.7 21.7 13.9 22.7 11.9 23.1 14.8 23.5 100.0 24.1 58.3 25.1 31.0 28.6 7.9 30.0 49.4 30.4 10.5 32.3 11.3 33.9 6.4 HCl Salt Form IV HCl salt Form IV was obtained via slurry of Compound 1 free Form I and equal molar HCl in THF at RT for 4 days and air-drying at RT overnight.
  • XRPD results are shown in Figure 33A and Table 46A.
  • TGA/DSC curves were shown in Figure 33B.
  • TGA showed a weight loss of 6.65% up to 150 oC.
  • DSC showed two exotherms at 91.6 oC, 160.2 oC and one endotherm at 178.5 oC (peak temperature).
  • NMR result showed 115 ME1 ⁇ 53438692.v1 136867-00920 that no solvent residue was detected.
  • UPLC and IC results confirmed that the purity was 97.13 area% and the stoichiometric ratio of Cl-/freeform was only 0.3.
  • UPLC results were shown in Figure 33D and Table 46B.
  • Table 46A Peaks list of HCl salt Form IV 2 ⁇ [°] Rel [%] 4.8 36.5 5.4 22.1 8.1 5.5 8.7 69.2 9.2 19.1 12.4 7.0 13.2 36.5 13.3 40.2 14.2 22.0 14.9 28.5 15.8 47.8 16.2 23.9 17.4 29.3 17.7 100.0 19.6 25.5 21.1 39.5 21.4 16.7 24.1 34.6 30.0 64.9
  • Table 46B UPLC result of HCl salt Form IV 116 ME1 ⁇ 53438692.v1 136867-00920 # Peak RRT Area% 1 0.52 2.60 2 1.00 97.13 3 1.37 0.05 4 1.43 0.13 5 1.60 0.08 While a number of embodiments have been described, the scope of this disclosure is to be defined by the appended claims, and not by the specific embodiments that have been represented by way of example.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

Abstract

Provided herein are crystalline salt forms of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one.

Description

136867-00920 CRYSTALLINE FORMS OF 3- FLUORO-2-(METHYLSULFAMOYLAMINO)-4- PYRIDYL]METHYL]-7-[(3- 2-PYRIDYL)OXY]-4-METHYL-CHROMEN- 2-ONE RELATED APPLICATIONS This application claims the benefit of priority to U.S. Provisional Application No. 63/659,793, filed June 13, 2024, the entire contents of each of which are incorporated herein by reference. BACKGROUND Cancer is among the most common causes of death in the United States. In the United States, cancer has accounted for approximately one of every four deaths. The 5-year relative survival rate for cancer patients diagnosed in 1996-2003 is approximately two-thirds, up from about one half in 1975-1977 (Cancer Facts & Figures, American Cancer Society: Atlanta, Ga. (2008)). The rate of new cancer cases decreased by an average 0.6% per year among men between 2000 and 2009, but stayed the same for women. From 2000 through 2009, death rates from all cancers combined decreased on average 1.8% per year among men and 1.4% per year among women. This improvement in survival reflects progress in diagnosing at an earlier stage as well as improvements in treatment, for which there remains a need. Discovering highly effective anticancer agents with low toxicity is a primary goal of cancer research. Mitogen-activated protein kinase (MEK) is a critical signaling intermediate in the MAPK/ERK pathway, which is inappropriately activated across a broad spectrum of human tumors, including those derived from lung, pancreas, ovary, skin and colon. While several MEK inhibitors have achieved regulatory approval to date, these MEK inhibitors have yet to deliver against clinical efficacy expectations, and combinations of these MEK inhibitors with RAF inhibitors are required to achieve more durable responses. Novel small molecules which act as dual inhibitors of MEK and extra cellular signal-regulated kinases (ERK) are described in PCT/US2023/019588. Of these compounds, 3-[[3-fluoro-2-(methylsulfamoylamino)-4- pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one, shows great therapeutic potential for treating a variety of conditions associated with the inhibition of MEK and/or ERK as it not only displays excellent potency, but it also has good CNS penetration and is effective against impeding the growth of multiple cancer cell lines. The 1 ME1\53438692.v1 136867-00920 development of alternative forms of this compound is therefore needed in an effort to e.g., facilitate isolation, manufacturing, and formulation development, as well as to maximize storage stability. SUMMARY Provided herein are salt forms (e.g., crystalline salt forms) of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen-2- one, hereinafter referred to as Compound 1. Also provided are pharmaceutical compositions comprising one or more salt forms of Compound 1 are also provided. Further provided are methods of preparing the described salt forms of Compound 1 as well as their use for treating conditions responsive to inhibition of MEK or ERK, or both, e.g., in a subject. Compound 1 and uses thereof are disclosed in International Application Serial No. PCT/US2023/019588, filed April 24, 2023, the entire teachings of which are incorporated herein by reference. BRIEF DESCRIPTION OF THE FIGURES FIGURE 1A depicts an X-ray powder diffraction pattern (XRPD) for potassium salt Form I of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one. FIGURE 1B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for potassium salt Form I of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. FIGURE 1C depicts the NMR spectrum for potassium salt Form I of 3-[[3-fluoro- 2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one. FIGURE 1D depicts the ultra performance liquid chromatography (hereinafter UPLC) results for potassium salt Form I of 3-[[3-fluoro-2-(methylsulfamoylamino)-4- pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one. 2 ME1\53438692.v1 136867-00920 FIGURE 1E depicts a variable temperature X-ray powder diffraction (hereinafter VT-XRPD) overlay pattern for potassium salt Form I of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. FIGURE 2A depicts an X-ray powder diffraction pattern (XRPD) for potassium salt Form II of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one. FIGURE 2B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for potassium salt Form II of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. FIGURE 2C depicts the NMR spectrum for potassium salt Form II of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one. FIGURE 2D depicts the UPLC results for potassium salt Form II of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. FIGURE 2E depicts a VT-XRPD overlay pattern for potassium salt Form II of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one. FIGURE 3A depicts an X-ray powder diffraction pattern (XRPD) for potassium salt Form III of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one. FIGURE 3B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for potassium salt Form III of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. FIGURE 3C depicts the NMR spectrum for potassium salt Form III of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one. FIGURE 3D depicts the UPLC results for potassium salt Form III of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 3 ME1\53438692.v1 136867-00920 FIGURE 3E depicts a VT-XRPD overlay pattern for potassium salt Form III of 3- [[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4- methyl-chromen-2-one. FIGURE 3F depicts a XRPD overlay pattern for potassium salt Forms I, II and III of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4- methyl-chromen-2-one. FIGURE 4A depicts an X-ray powder diffraction pattern (XRPD) for sodium salt Form II of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one. FIGURE 4B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for sodium salt Form II of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. FIGURE 4C depicts the NMR spectrum for sodium salt Form II of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. FIGURE 4D depicts the UPLC results for sodium salt Form II of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. FIGURE 4E depicts a VT-XRPD overlay pattern for sodium salt Form II of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one. FIGURE 4F depicts a XRPD overlay pattern for sodium salt Forms I and II of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one, before and after drying. FIGURE 4G depicts a XRPD overlay pattern for sodium salt Forms I to VII of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one. FIGURE 4H depicts an X-ray powder diffraction pattern (XRPD) for sodium salt Form I of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one. 4 ME1\53438692.v1 136867-00920 FIGURE 5A depicts an X-ray powder diffraction pattern (XRPD) for sodium salt Form III of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one. FIGURE 5B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for sodium salt Form III of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. FIGURE 5C depicts the NMR spectrum for sodium salt Form III of 3-[[3-fluoro- 2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one. FIGURE 5D depicts the UPLC results for sodium salt Form III of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. FIGURE 6 depicts an X-ray powder diffraction pattern (XRPD) for sodium salt Form IV of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]- 4-methyl-chromen-2-one. FIGURE 7A depicts an X-ray powder diffraction pattern (XRPD) for sodium salt Form V of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one. FIGURE 7B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for sodium salt Form V of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. FIGURE 7C depicts the NMR spectrum for sodium salt Form V of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. FIGURE 7D depicts the UPLC results for sodium salt Form V of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. FIGURE 7E depicts a VT-XRPD overlay pattern for sodium salt Form V of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one. 5 ME1\53438692.v1 136867-00920 FIGURE 8A depicts an X-ray powder diffraction pattern (XRPD) for sodium salt Form VI of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one. FIGURE 8B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for sodium salt Form VI of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. FIGURE 8C depicts the NMR spectrum for sodium salt Form VI of 3-[[3-fluoro- 2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one. FIGURE 8D depicts the UPLC results for sodium salt Form VI of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. FIGURE 9A depicts an X-ray powder diffraction pattern (XRPD) for sodium salt Form VII of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one. FIGURE 9B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for sodium salt Form VII of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. FIGURE 9C depicts the NMR spectrum for sodium salt Form VII of 3-[[3-fluoro- 2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one. FIGURE 9D depicts the UPLC results for sodium salt Form VII of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. FIGURE 9E depicts a VT-XRPD overlay pattern for sodium salt Form VII of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one. FIGURE 10A depicts an X-ray powder diffraction pattern (XRPD) for calcium salt Form I of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one. 6 ME1\53438692.v1 136867-00920 FIGURE 10B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for calcium salt Form I of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. FIGURE 10C depicts the NMR spectrum for calcium salt Form I of 3-[[3-fluoro- 2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one. FIGURE 10D depicts the UPLC results for calcium salt Form I of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. FIGURE 10E depicts a VT-XRPD overlay pattern for calcium salt Form I of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one. FIGURE 10F depicts a XRPD overlay pattern for calcium salt Forms I to V of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one. FIGURE 11A depicts an X-ray powder diffraction pattern (XRPD) for calcium salt Form II of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one. FIGURE 11B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for calcium salt Form II of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. FIGURE 11C depicts the NMR spectrum for calcium salt Form II of 3-[[3-fluoro- 2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one. FIGURE 11D depicts the UPLC results for calcium salt Form II of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. FIGURE 11E depicts a VT-XRPD overlay pattern for calcium salt Form II of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one. 7 ME1\53438692.v1 136867-00920 FIGURE 12A depicts an X-ray powder diffraction pattern (XRPD) for calcium salt Form III of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one. FIGURE 12B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for calcium salt Form III of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. FIGURE 12C depicts the NMR spectrum for calcium salt Form III of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one. FIGURE 12D depicts the UPLC results for calcium salt Form III of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. FIGURE 12E depicts a VT-XRPD overlay pattern for calcium salt Form III of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one. FIGURE 13A depicts an X-ray powder diffraction pattern (XRPD) for calcium salt Form IV of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one. FIGURE 13B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for calcium salt Form IV of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. FIGURE 13C depicts the NMR spectrum for calcium salt Form IV of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one. FIGURE 13D depicts the UPLC results for calcium salt Form IV of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. FIGURE 13E depicts an XRPD overlay pattern for calcium salt Form IV of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one, before and after storage. 8 ME1\53438692.v1 136867-00920 FIGURE 13F depicts a VT-XRPD overlay pattern for calcium salt Form V of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one. FIGURE 14 depicts an X-ray powder diffraction pattern (XRPD) for calcium salt Form V of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one. FIGURE 15A depicts an X-ray powder diffraction pattern (XRPD) for Choline salt Form I of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one. FIGURE 15B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for Choline salt Form I of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. FIGURE 15C depicts the NMR spectrum for Choline salt Form I of 3-[[3-fluoro- 2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one. FIGURE 15D depicts the UPLC results for Choline salt Form I of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. FIGURE 15E depicts a VT-XRPD overlay pattern for Choline salt Form I of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one. FIGURE 15F depicts a XRPD overlay pattern for Choline salt Forms I - VI of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one. FIGURE 16A depicts an X-ray powder diffraction pattern (XRPD) for Choline salt Form II of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one. FIGURE 16B depicts an XRPD overlay pattern for Choline salt Form II of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one, before and after drying. 9 ME1\53438692.v1 136867-00920 FIGURE 17A depicts an X-ray powder diffraction pattern (XRPD) for choline salt Form III of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one. FIGURE 17B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for Choline salt Form III of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. FIGURE 17C depicts the NMR spectrum for Choline salt Form III of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one. FIGURE 17D depicts the UPLC results for Choline salt Form III of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. FIGURE 17E depicts a VT-XRPD overlay pattern for Choline salt Form III of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one. FIGURE 18A depicts an X-ray powder diffraction pattern (XRPD) for choline salt Form IV of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one. FIGURE 18B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for choline salt Form IV of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. FIGURE 18C depicts the NMR spectrum for Choline salt Form IV of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one. FIGURE 18D depicts the UPLC results for Choline salt Form IV of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. FIGURE 18E depicts a VT-XRPD overlay pattern for Choline salt Form IV of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one. 10 ME1\53438692.v1 136867-00920 FIGURE 19A depicts an X-ray powder diffraction pattern (XRPD) for choline salt Form V of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one. FIGURE 19B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for choline salt Form V of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. FIGURE 19C depicts the NMR spectrum for Choline salt Form V of 3-[[3-fluoro- 2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one. FIGURE 19D depicts the UPLC results for Choline salt Form V of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. FIGURE 20A depicts an X-ray powder diffraction pattern (XRPD) for choline salt Form VI of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one. FIGURE 20B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for choline salt Form VI of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. FIGURE 20C depicts the NMR spectrum for Choline salt Form VI of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one. FIGURE 20D depicts the UPLC results for Choline salt Form VI of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. FIGURE 21A depicts an X-ray powder diffraction pattern (XRPD) for hydrogen bromide salt Form I of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3- fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one. FIGURE 21B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for hydrogen bromide salt Form I of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. 11 ME1\53438692.v1 136867-00920 FIGURE 21C depicts the 1H NMR spectrum for hydrogen bromide salt Form I of 3- [[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4- methyl-chromen-2-one. FIGURE 21D depicts the UPLC results for hydrogen bromide salt Form I of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one. FIGURE 21E depicts a XRPD overlay pattern for hydrogen bromide salt Forms I-III of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4- methyl-chromen-2-one. FIGURE 22A depicts an X-ray powder diffraction pattern (XRPD) for hydrogen bromide salt Form II of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3- fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one. FIGURE 22B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for hydrogen bromide salt Form II of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. FIGURE 22C depicts the NMR spectrum for hydrogen bromide salt Form II of 3- [[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4- methyl-chromen-2-one. FIGURE 22D depicts the UPLC results for hydrogen bromide salt Form II of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one. FIGURE 22E depicts a VT-XRPD overlay pattern for hydrogen bromide salt Form II of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4- methyl-chromen-2-one. FIGURE 23A depicts an X-ray powder diffraction pattern (XRPD) for hydrogen bromide salt Form III of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3- fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one. FIGURE 23B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for hydrogen bromide salt Form III of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. 12 ME1\53438692.v1 136867-00920 FIGURE 24A depicts an X-ray powder diffraction pattern (XRPD) for 1,5- naphthalenedisulfonate salt Form I of 3-[[3-fluoro-2-(methylsulfamoylamino)-4- pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one. FIGURE 24B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for 1,5-naphthalenedisulfonate salt Form I of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. FIGURE 24C depicts the NMR spectrum for naphthalenedisulfonate salt Form I of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4- methyl-chromen-2-one. FIGURE 24D depicts the UPLC results for naphthalenedisulfonate salt Form I of 3- [[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4- methyl-chromen-2-one. FIGURE 25A depicts an X-ray powder diffraction pattern (XRPD) for 1,5- naphthalenedisulfonate salt Form II of 3-[[3-fluoro-2-(methylsulfamoylamino)-4- pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one. FIGURE 25B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for 1,5-naphthalenedisulfonate salt Form II of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. FIGURE 25C depicts the NMR spectrum for naphthalenedisulfonate salt Form II of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4- methyl-chromen-2-one. FIGURE 25D depicts the UPLC results for naphthalenedisulfonate salt Form II of 3- [[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4- methyl-chromen-2-one. FIGURE 26A depicts an X-ray powder diffraction pattern (XRPD) for edisylate salt Form I of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one. FIGURE 26B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for edisylate salt Form I of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. 13 ME1\53438692.v1 136867-00920 FIGURE 26C depicts the 1H NMR spectrum for edisylate salt Form I of 3-[[3-fluoro- 2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one. FIGURE 26D depicts the UPLC results for edisylate salt Form I of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. FIGURE 27A depicts an X-ray powder diffraction pattern (XRPD) for edisylate salt Form II of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one. FIGURE 27B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for edisylate salt Form II of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. FIGURE 27C depicts the NMR spectrum for edisylate salt Form II of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one. FIGURE 27D depicts the UPLC results for edisylate salt Form II of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. FIGURE 28A depicts an X-ray powder diffraction pattern (XRPD) for diethylamine salt Form I of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one. FIGURE 28B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for diethylamine salt Form I of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. FIGURE 28C depicts the NMR spectrum for diethylamine salt Form I of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one. FIGURE 28D depicts the UPLC results for diethylamine salt Form I of 3-[[3-fluoro- 2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one. 14 ME1\53438692.v1 136867-00920 FIGURE 28E depicts a VT-XRPD overlay pattern for diethylamine salt Form I of 3- [[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4- methyl-chromen-2-one. FIGURE 29A depicts an X-ray powder diffraction pattern (XRPD) for diethylamine salt Form II of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one. FIGURE 29B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for diethylamine salt Form II of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. FIGURE 29C depicts the NMR spectrum for diethylamine salt Form II of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one. FIGURE 29D depicts the UPLC results for diethylamine salt Form II of 3-[[3-fluoro- 2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one. FIGURE 29E depicts a VT-XRPD overlay pattern for diethylamine salt Form II of 3- [[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4- methyl-chromen-2-one. FIGURE 30A depicts an X-ray powder diffraction pattern (XRPD) for hydrogen chloride salt Form I of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3- fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one. FIGURE 30B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for hydrogen chloride salt Form I of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. FIGURE 30C depicts the NMR spectrum for hydrogen chloride salt Form I of 3- [[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4- methyl-chromen-2-one. FIGURE 30D depicts the UPLC results for hydrogen chloride salt Form I of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one. 15 ME1\53438692.v1 136867-00920 FIGURE 31 depicts an X-ray powder diffraction pattern (XRPD) for hydrogen chloride salt Form II of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3- fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one. FIGURE 32 depicts an X-ray powder diffraction pattern (XRPD) for hydrogen chloride salt Form III of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3- fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one. FIGURE 33A depicts an X-ray powder diffraction pattern (XRPD) for hydrogen chloride salt Form IV of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3- fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one. FIGURE 33B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for hydrogen chloride salt Form IV of 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. FIGURE 33C depicts the NMR spectrum for hydrogen chloride salt Form IV of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4- methyl-chromen-2-one. FIGURE 33D depicts the UPLC results for hydrogen chloride salt Form IV of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one. FIGURE 33E depicts a XRPD overlay pattern for hydrogen chloride salt Form IV of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4- methyl-chromen-2-one, before and after drying. FIGURE 34A depicts X-ray powder diffraction (XRPD) patterns for reference sample free Form I of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3- fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one, and for the solid starting material used in salt screening described in the present disclosure. FIGURE 34B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for reference sample free Form I , the solid starting material used in salt screening described in the present disclosure. FIGURE 35A depicts X-ray powder diffraction (XRPD) overlay patterns for reference sample potassium salt Form I of 3-[[3-fluoro-2-(methylsulfamoylamino)-4- pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one, and for the re- prepared sample of potassium salt Form I. 16 ME1\53438692.v1 136867-00920 FIGURE 35B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for the re-prepared sample of potassium salt Form I of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one. FIGURE 36A depicts X-ray powder diffraction (XRPD) overlay patterns for reference sample sodium salt Form II of 3-[[3-fluoro-2-(methylsulfamoylamino)-4- pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one, and for the re- prepared sample of sodium salt Form II. FIGURE 36B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for the re-prepared sample of sodium salt Form II of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one. FIGURE 37A depicts X-ray powder diffraction (XRPD) overlay patterns for reference sample calcium salt Form II of 3-[[3-fluoro-2-(methylsulfamoylamino)-4- pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one, and for the re- prepared sample of calcium salt Form II. FIGURE 37B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for the re-prepared sample of calcium salt Form II of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one. FIGURE 38A depicts X-ray powder diffraction (XRPD) overlay patterns for reference sample choline salt Form I of 3-[[3-fluoro-2-(methylsulfamoylamino)-4- pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one, and for the re- prepared sample of choline salt Form I. FIGURE 38B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for the re-prepared sample of choline salt Form I of 3-[[3- fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl- chromen-2-one. FIGURE 39A depicts X-ray powder diffraction (XRPD) overlay patterns for reference sample hydrogen bromide salt Form II of 3-[[3-fluoro-2-(methylsulfamoylamino)- 4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one, and for the re- prepared sample of hydrogen bromide salt Form II. 17 ME1\53438692.v1 136867-00920 FIGURE 39B depicts differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) thermograms for the re-prepared sample of hydrogen bromide salt Form II of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4- methyl-chromen-2-one. FIGURE 40 depicts structures of selected the counter-ions/co-formers used in the salt screening experiments. DETAILED DESCRIPTION Provided are salt forms of Compound 1. “Compound 1” and 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one are used interchangeably, and each refer to the compound having the following chemical structure: . As used herein, “crystalline” refers to a solid form of a compound wherein there exists long-range atomic order in the positions of the atoms. The crystalline nature of a solid can be confirmed, for example, by examination of the X-ray powder diffraction pattern. A salt can be a solvate or anhydrate. “Solvate” refers to a salt form which incorporates solvent within the three dimensional configuration; commonly a stoichiometric amount of solvent relative to Compound 1 is incorporated within the three dimensional configuration. “Hydrate” refers to a solvate wherein the solvent is water. “Anhydrate” refers to a salt form that is characterized by the substantial absence water, e.g., less than 1% by weight as determined by Karl Fisher analysis, within the crystal structure. “Substantial absence of solvent” within the crystal structure includes less than 0.25 molar equivalents, and less than 0.1 molar equivalents of solvent relative to Compound 1. In one embodiment, the salts of Compound 1 described herein are selected from potassium salts, sodium salts, calcium salts, choline salts, hydrogen bromide salts, 1,5- naphthalenedisulfonate salts, edisylate salts, diethylamine salts, and hydrogen chloride salts. In another embodiment, the salts of Compound 1 described herein are selected from potassium salt Forms I, II, and III; sodium salt Forms II, III, IV, V, VI, and VII; calcium salt Forms I, II, III, IV, and V; choline salt Forms I, II, III, IV, V, and VI; hydrogen bromide salt 18 ME1\53438692.v1 136867-00920 Forms I, II, and III; 1,5-naphthalenedisulfonate salt Forms I and II; edisylate salt Forms I and II, diethylamine salt Forms I and II; and hydrogen chloride salt Forms I, II, III, and IV. In one embodiment, the salts of Compound 1 described herein are crystalline. In one embodiment, the salts of Compound 1 are each a single crystalline form. A “single crystalline form” means that the recited compound, i.e., Compound 1, is present as a single crystal or a plurality of crystals in which each crystal has the same crystal form (e.g., Form I or Form II). Percent by weight of a particular crystal form is determined by the weight of the particular crystal form divided by the sum weight of the particular crystal, plus the weight of the other crystal form(s) present plus the weight of amorphous form, if present, multiplied by 100%. In some instances, each crystalline form as described herein is at least 60%, at least 70%, at least 80%, at least 90%, at least 95%, or at least 99% a single crystalline form. “Pure single crystalline form” means that Compound 1 is present as a single crystal or a plurality of crystals in which each crystal has the same crystal form with no other detectable amounts of other crystal forms present and/or amorphous forms. The term “amorphous” refers to a solid that is present in a non-crystalline state or form. Amorphous solids are disordered arrangements of molecules and therefore possess no distinguishable crystal lattice or unit cell and consequently have no definable long range ordering. Solid state ordering of solids may be determined by standard techniques known in the art, e.g., by X-ray powder diffraction (XRPD) or differential scanning calorimetry (DSC). The 2-theta (2θ) values of the X-ray powder diffraction patterns for the crystalline forms described herein may vary slightly from one instrument to another and also depending on variations in sample preparation and batch to batch variation due to factors such as temperature variation, sample displacement, and the presence or absence of an internal standard. Therefore, unless otherwise defined, the XRPD patterns / assignments recited herein are not to be construed as absolute and can vary ± 0.2 degrees. It is well known in the art that this variability will account for the above factors without hindering the unequivocal identification of a crystal form. Unless otherwise specified, the 2-theta values provided herein were obtained using Cu Kα1 radiation. "Substantially the same XRPD pattern” or “an X-ray powder diffraction pattern substantially similar to” a defined figure means that for comparison purposes, at least 90% of the peaks shown are present. It is to be further understood that for comparison purposes some variability in peak intensities from those shown are allowed, such as ± 5% of the intensity of the most intense peak. 19 ME1\53438692.v1 136867-00920 Temperature values, e.g., for DSC peaks herein may vary slightly from one instrument to another and also depending on variations in sample preparation, batch to batch variation, and environmental factors. Therefore, unless otherwise defined, temperature values recited herein are not to be construed as absolute and can vary ± 5 degrees or ± 2 degrees Celsius. Potassium Salt Form I In one embodiment, potassium salt crystalline Form I is characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 4.5°, 8.9°, 14.6°, 17.2°, 17.8°, 23.5°, and 23.8°. In another embodiment, potassium salt crystalline Form I is characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 4.5°, 8.9°, 14.6°, 17.2°, 17.8°, 23.5°, and 23.8°. In another embodiment, potassium salt crystalline Form I is characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 4.5°, 8.9°, 14.6°, 17.2°, 17.8°, 23.5°, and 23.8°. In another embodiment, potassium salt crystalline Form I is characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 4.5°, 8.9°, 14.6°, 17.2°, 17.8°, 23.5°, and 23.8°. In another embodiment, potassium salt crystalline Form I is characterized by x-ray powder diffraction peaks at 2θ angles 4.5°, 8.9°, 14.6°, 17.2°, 17.8°, 23.5°, and 23.8°. In another embodiment, potassium salt crystalline Form I is characterized by at least three, four, five, six, or all x-ray powder diffraction peaks at 2θ angles selected from 4.5°, 8.9°, 14.6°, 17.2°, 17.8°, 23.5°, and 23.8°, and is further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 7.3°, 10.6°, 19.3°, 22.1°, and 22.4°. In another embodiment, potassium salt crystalline Form I is characterized by one or more, or all of the x-ray powder diffraction peaks at 2θ angles provided in Table 11A. In another embodiment, potassium salt crystalline Form I is characterized by an x-ray powder diffraction substantially similar to Figure 1A. In another embodiment, potassium salt crystalline Form I is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 1A, or the peaks recited in Table 11A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising a peak endotherm at 246.1 °C ± 2 °C. In another embodiment, the molar ratio of potassium counter-ion to compound in potassium salt crystalline Form I is about 0.9, and potassium salt crystalline Form I is further characterized by the features in any one of the previous two paragraphs, Figure 1A, or the peaks recited in Table 11A. 20 ME1\53438692.v1 136867-00920 In another embodiment, potassium salt crystalline Form I is an anhydrate, and is further characterized by the features in any one of the previous three paragraphs, Figure 1A, or the peaks recited in Table 11A. Potassium Salt Form II In one embodiment, potassium salt crystalline Form II is characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 4.4°, 8.6°, 14.4°, 17.5°, 18.4°, 21.5°, and 24.0°. In another embodiment, potassium salt crystalline Form II is characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 4.4°, 8.6°, 14.4°, 17.5°, 18.4°, 21.5°, and 24.0°. In another embodiment, potassium salt crystalline Form II is characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 4.4°, 8.6°, 14.4°, 17.5°, 18.4°, 21.5°, and 24.0°. In another embodiment, potassium salt crystalline Form II is characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 4.4°, 8.6°, 14.4°, 17.5°, 18.4°, 21.5°, and 24.0°. In another embodiment, potassium salt crystalline Form II is characterized by x-ray powder diffraction peaks at 2θ angles 4.4°, 8.6°, 14.4°, 17.5°, 18.4°, 21.5°, and 24.0°. In another embodiment, potassium salt crystalline Form II is characterized by at least three, four, five, six, or all x-ray powder diffraction peaks at 2θ angles selected from 4.4°, 8.6°, 14.4°, 17.5°, 18.4°, 21.5°, and 24.0°, and is further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 7.8°, 17.2°, 18.9°, 23.5°, and 27.6°. In another embodiment, potassium salt crystalline Form II is characterized by one or more, or all of the x-ray powder diffraction peaks at 2θ angles provided in Table 12A. In another embodiment, potassium salt crystalline Form II is characterized by an x-ray powder diffraction substantially similar to Figure 2A. In another embodiment, potassium salt crystalline Form II is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 2A, or the peaks recited in Table 12A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising a peak endotherm at 257.9 °C ± 2 °C. In another embodiment, the molar ratio of potassium counter-ion to compound in potassium salt crystalline Form II is about 1, and potassium salt crystalline Form II is further characterized by the features in any one of the previous two paragraphs, Figure 2A, or the peaks recited in Table 12A. In another embodiment, potassium salt crystalline Form II is an anhydrate, and is further characterized by the features in any one of the previous three paragraphs, Figure 2A, or the peaks recited in Table 12A. 21 ME1\53438692.v1 136867-00920 Potassium Salt Form III In one embodiment, potassium salt crystalline Form III is characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 7.2°, 9.3°, 10.2°, 13.6°, 15.0°, 17.0°, and 20.4°. In another embodiment, potassium salt crystalline Form III is characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 7.2°, 9.3°, 10.2°, 13.6°, 15.0°, 17.0°, and 20.4°. In another embodiment, potassium salt crystalline Form III is characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 7.2°, 9.3°, 10.2°, 13.6°, 15.0°, 17.0°, and 20.4°. In another embodiment, potassium salt crystalline Form III is characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 7.2°, 9.3°, 10.2°, 13.6°, 15.0°, 17.0°, and 20.4°. In another embodiment, potassium salt crystalline Form III is characterized by x-ray powder diffraction peaks at 2θ angles 7.2°, 9.3°, 10.2°, 13.6°, 15.0°, 17.0°, and 20.4°. In another embodiment, potassium salt crystalline Form III is characterized by at least three, four, five, six, or all x-ray powder diffraction peaks at 2θ angles selected from 7.2°, 9.3°, 10.2°, 13.6°, 15.0°, 17.0°, and 20.4°, and is further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 12.0°, 13.2°, 17.7°, and 23.9°. In another embodiment, potassium salt crystalline Form III is characterized by one or more, or all of the x-ray powder diffraction peaks at 2θ angles provided in Table 13A. In another embodiment, potassium salt crystalline Form III is characterized by an x-ray powder diffraction substantially similar to Figure 3A. In another embodiment, potassium salt crystalline Form III is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 3A, or the peaks recited in Table 13A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 149.0 °C, 161.3 °C, and 267.5 °C ± 2 °C. In another embodiment, the molar ratio of potassium counter-ion to compound in potassium salt crystalline Form III is about 0.9, and potassium salt crystalline Form III is further characterized by the features in any one of the previous two paragraphs, Figure 3A, or the peaks recited in Table 13A. In another embodiment, potassium salt crystalline Form III is a DMSO solvate, and is further characterized by the features in any one of the previous three paragraphs, Figure 3A, or the peaks recited in Table 13A. Sodium Salt Form II In one embodiment, sodium salt crystalline Form II is characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 6.5°, 7.6°, 14.7°, 15.2°, and 22.9°. 22 ME1\53438692.v1 136867-00920 In another embodiment, sodium salt crystalline Form II is characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 6.5°, 7.6°, 14.7°, 15.2°, and 22.9°. In another embodiment, sodium salt crystalline Form II is characterized by x-ray powder diffraction peaks at 2θ angles 6.5°, 7.6°, 14.7°, 15.2°, and 22.9°. In another embodiment, sodium salt crystalline Form II is characterized by at least three, four, or all x-ray powder diffraction peaks at 2θ angles selected from 6.5°, 7.6°, 14.7°, 15.2°, and 22.9°, and is further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 8.4°, 17.1°, and 18.0°. In another embodiment, sodium salt crystalline Form II is characterized by one or more, or all of the x-ray powder diffraction peaks at 2θ angles provided in Table 15A. In another embodiment, sodium salt crystalline Form II is characterized by an x-ray powder diffraction substantially similar to Figure 4A. In another embodiment, sodium salt crystalline Form II is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 4A, or the peaks recited in Table 15A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 65.3 °C, 118.5 °C, and 179.3 °C ± 2 °C. In another embodiment, the molar ratio of sodium counter-ion to compound in sodium salt crystalline Form II is about 1.1, and sodium salt crystalline Form II is further characterized by the features in any one of the previous two paragraphs, Figure 4A, or the peaks recited in Table 15A. In another embodiment, sodium salt crystalline Form II is a hydrate, and is further characterized by the features in any one of the previous three paragraphs, Figure 4A, or the peaks recited in Table 15A. Sodium Salt Form III In one embodiment, sodium salt crystalline Form III is characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 9.7°, 9.9°, 15.3°, 17.8°, 18.6°, 19.0°, 22.9°, and 23.6°. In another embodiment, sodium salt crystalline Form III is characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 9.7°, 9.9°, 15.3°, 17.8°, 18.6°, 19.0°, 22.9°, and 23.6°. In another embodiment, sodium salt crystalline Form III is characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 9.7°, 9.9°, 15.3°, 17.8°, 18.6°, 19.0°, 22.9°, and 23.6°. In another embodiment, sodium salt crystalline Form III is characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 9.7°, 9.9°, 15.3°, 17.8°, 18.6°, 19.0°, 22.9°, and 23.6°. In another embodiment, sodium salt crystalline Form III is characterized by at least 23 ME1\53438692.v1 136867-00920 seven x-ray powder diffraction peaks at 2θ angles selected from 9.7°, 9.9°, 15.3°, 17.8°, 18.6°, 19.0°, 22.9°, and 23.6°. In another embodiment, sodium salt crystalline Form III is characterized by x-ray powder diffraction peaks at 2θ angles 9.7°, 9.9°, 15.3°, 17.8°, 18.6°, 19.0°, 22.9°, and 23.6°. In another embodiment, sodium salt crystalline Form III is characterized by at least three, four, five, six, seven, or all x-ray powder diffraction peaks at 2θ angles selected from 9.7°, 9.9°, 15.3°, 17.8°, 18.6°, 19.0°, 22.9°, and 23.6°, and is further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 13.2°, 15.6°, 16.4°, 16.6°, 21.0°, 22.0°, and 22.5°. In another embodiment, sodium salt crystalline Form III is characterized by one or more, or all of the x-ray powder diffraction peaks at 2θ angles provided in Table 16A. In another embodiment, sodium salt crystalline Form III is characterized by an x-ray powder diffraction substantially similar to Figure 5A. In another embodiment, sodium salt crystalline Form III is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 5A, or the peaks recited in Table 16A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising a peak endotherm at 179.8 °C ± 2 °C. In another embodiment, the molar ratio of sodium counter-ion to compound in sodium salt crystalline Form III is about 1.1, and sodium salt crystalline Form III is further characterized by the features in any one of the previous two paragraphs, Figure 5A, or the peaks recited in Table 16A. In another embodiment, sodium salt crystalline Form III is a DMSO solvate, and is further characterized by the features in any one of the previous three paragraphs, Figure 5A, or the peaks recited in Table 16A. Sodium Salt Form IV In one embodiment, sodium salt crystalline Form IV is characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 8.0°, 12.3°, 14.5°, 14.9°, 15.2°, 16.0°, and 24.7°. In another embodiment, sodium salt crystalline Form IV is characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 8.0°, 12.3°, 14.5°, 14.9°, 15.2°, 16.0°, and 24.7°. In another embodiment, sodium salt crystalline Form IV is characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 8.0°, 12.3°, 14.5°, 14.9°, 15.2°, 16.0°, and 24.7°. In another embodiment, sodium salt crystalline Form IV is characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 8.0°, 12.3°, 14.5°, 14.9°, 15.2°, 16.0°, and 24.7°. In another embodiment, sodium salt crystalline Form IV is characterized by x-ray powder diffraction peaks at 2θ angles 8.0°, 24 ME1\53438692.v1 136867-00920 12.3°, 14.5°, 14.9°, 15.2°, 16.0°, and 24.7°. In another embodiment, sodium salt crystalline Form IV is characterized by at least three, four, five, six, or all x-ray powder diffraction peaks at 2θ angles selected from 8.0°, 12.3°, 14.5°, 14.9°, 15.2°, 16.0°, and 24.7°, and is further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 13.3°, 17.7°, 22.1°, 23.0°, and 29.4°. In another embodiment, sodium salt crystalline Form IV is characterized by one or more, or all of the x-ray powder diffraction peaks at 2θ angles provided in Table 17. In another embodiment, sodium salt crystalline Form IV is characterized by an x-ray powder diffraction substantially similar to Figure 6. Sodium Salt Form V In one embodiment, sodium salt crystalline Form V is characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 9.6°, 10.8°, 16.2°, 17.5°, 19.7°, 22.1°, 23.3°, and 24.3°. In another embodiment, sodium salt crystalline Form V is characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 9.6°, 10.8°, 16.2°, 17.5°, 19.7°, 22.1°, 23.3°, and 24.3°. In another embodiment, sodium salt crystalline Form V is characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 9.6°, 10.8°, 16.2°, 17.5°, 19.7°, 22.1°, 23.3°, and 24.3°. In another embodiment, sodium salt crystalline Form V is characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 9.6°, 10.8°, 16.2°, 17.5°, 19.7°, 22.1°, 23.3°, and 24.3°. In another embodiment, sodium salt crystalline Form V is characterized by at least seven x-ray powder diffraction peaks at 2θ angles selected from 9.6°, 10.8°, 16.2°, 17.5°, 19.7°, 22.1°, 23.3°, and 24.3°. In another embodiment, sodium salt crystalline Form V is characterized by x-ray powder diffraction peaks at 2θ angles 9.6°, 10.8°, 16.2°, 17.5°, 19.7°, 22.1°, 23.3°, and 24.3°. In another embodiment, sodium salt crystalline Form V is characterized by at least three, four, five, six, seven, or all x-ray powder diffraction peaks at 2θ angles selected from 9.6°, 10.8°, 16.2°, 17.5°, 19.7°, 22.1°, 23.3°, and 24.3°, and is further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 14.6°, 16.9°, 17.2°, 17.9°, 18.4°, 19.0°, 23.5°, and 29.5°. In another embodiment, sodium salt crystalline Form V is characterized by one or more, or all of the x-ray powder diffraction peaks at 2θ angles provided in Table 18A. In another embodiment, sodium salt crystalline Form V is characterized by an x-ray powder diffraction substantially similar to Figure 7A. In another embodiment, sodium salt crystalline Form V is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 7A, or the peaks recited in Table 25 ME1\53438692.v1 136867-00920 18A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 112.0 °C and 134.8 °C ± 2 °C. In another embodiment, the molar ratio of sodium counter-ion to compound in sodium salt crystalline Form V is about 1.0, and sodium salt crystalline Form V is further characterized by the features in any one of the previous two paragraphs, Figure 7A, or the peaks recited in Table 18A. In another embodiment, sodium salt crystalline Form V is a H2O-NMP co-solvate, and is further characterized by the features in any one of the previous three paragraphs, Figure 7A, or the peaks recited in Table 18A. Sodium Salt Form VI In one embodiment, sodium salt crystalline Form VI is characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 8.5°, 10.6°, 14.4°, 16.2°, 19.3°, 19.6°, 22.9°, and 23.3°. In another embodiment, sodium salt crystalline Form VI is characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 8.5°, 10.6°, 14.4°, 16.2°, 19.3°, 19.6°, 22.9°, and 23.3°. In another embodiment, sodium salt crystalline Form VI is characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 8.5°, 10.6°, 14.4°, 16.2°, 19.3°, 19.6°, 22.9°, and 23.3°. In another embodiment, sodium salt crystalline Form VI is characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 8.5°, 10.6°, 14.4°, 16.2°, 19.3°, 19.6°, 22.9°, and 23.3°. In another embodiment, sodium salt crystalline Form VI is characterized by at least seven x-ray powder diffraction peaks at 2θ angles selected from 8.5°, 10.6°, 14.4°, 16.2°, 19.3°, 19.6°, 22.9°, and 23.3°. In another embodiment, sodium salt crystalline Form VI is characterized by x-ray powder diffraction peaks at 2θ angles 8.5°, 10.6°, 14.4°, 16.2°, 19.3°, 19.6°, 22.9°, and 23.3°. In another embodiment, sodium salt crystalline Form VI is characterized by at least three, four, five, six, seven, or all x-ray powder diffraction peaks at 2θ angles selected from 8.5°, 10.6°, 14.4°, 16.2°, 19.3°, 19.6°, 22.9°, and 23.3°, and is further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 6.4°, 6.7°, 9.7°, 12.9°, 15.2°, 17.2°, 18.3°, 20.4°, 21.4°, and 29.0°. In another embodiment, sodium salt crystalline Form VI is characterized by one or more, or all of the x-ray powder diffraction peaks at 2θ angles provided in Table 19A. In another embodiment, sodium salt crystalline Form VI is characterized by an x-ray powder diffraction substantially similar to Figure 8A. In another embodiment, sodium salt crystalline Form VI is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 8A, or the peaks recited in Table 26 ME1\53438692.v1 136867-00920 19A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 49.9 °C, 100.2 °C, 116.9 °C, and 154.6 °C ± 2 °C. In another embodiment, the molar ratio of sodium counter-ion to compound in sodium salt crystalline Form VI is about 1.0, and sodium salt crystalline Form VI is further characterized by the features in any one of the previous two paragraphs, Figure 8A, or the peaks recited in Table 19A. In another embodiment, sodium salt crystalline Form VI is a DMAc solvate, and is further characterized by the features in any one of the previous three paragraphs, Figure 8A, or the peaks recited in Table 19A. Sodium Salt Form VII In one embodiment, sodium salt crystalline Form VII is characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 9.6°, 9.9°, 15.5°, 17.2°, 18.1°, 22.3°, 23.2°, and 29.0°. In another embodiment, sodium salt crystalline Form VII is characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 9.6°, 9.9°, 15.5°, 17.2°, 18.1°, 22.3°, 23.2°, and 29.0°. In another embodiment, sodium salt crystalline Form VII is characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 9.6°, 9.9°, 15.5°, 17.2°, 18.1°, 22.3°, 23.2°, and 29.0°. In another embodiment, sodium salt crystalline Form VII is characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 9.6°, 9.9°, 15.5°, 17.2°, 18.1°, 22.3°, 23.2°, and 29.0°. In another embodiment, sodium salt crystalline Form VII is characterized by at least seven x-ray powder diffraction peaks at 2θ angles selected from 9.6°, 9.9°, 15.5°, 17.2°, 18.1°, 22.3°, 23.2°, and 29.0°. In another embodiment, sodium salt crystalline Form VII is characterized by x-ray powder diffraction peaks at 2θ angles 9.6°, 9.9°, 15.5°, 17.2°, 18.1°, 22.3°, 23.2°, and 29.0°. In another embodiment, sodium salt crystalline Form VII is characterized by at least three, four, five, six, seven, or all x-ray powder diffraction peaks at 2θ angles selected from 9.6°, 9.9°, 15.5°, 17.2°, 18.1°, 22.3°, 23.2°, and 29.0°, and is further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 12.9°, 19.2°, 19.8°, 21.5°, 31.1°, and 32.0°. In another embodiment, sodium salt crystalline Form VII is characterized by one or more, or all of the x-ray powder diffraction peaks at 2θ angles provided in Table 20A. In another embodiment, sodium salt crystalline Form VII is characterized by an x-ray powder diffraction substantially similar to Figure 9A. In another embodiment, sodium salt crystalline Form VII is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 9A, or the peaks recited in Table 27 ME1\53438692.v1 136867-00920 20A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 154.7 °C, and 184.2 °C ± 2 °C. In another embodiment, the molar ratio of sodium counter-ion to compound in sodium salt crystalline Form VII is about 1.0, and sodium salt crystalline Form VII is further characterized by the features in any one of the previous two paragraphs, Figure 9A, or the peaks recited in Table 20A. In another embodiment, sodium salt crystalline Form VII is an acetone solvate, and is further characterized by the features in any one of the previous three paragraphs, Figure 9A, or the peaks recited in Table 20A. Calcium Salt Form I In one embodiment, calcium salt crystalline Form I is characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 6.4°, 7.0°, 12.5°, 14.0°, 17.3°, 18.0°, and 23.3°. In another embodiment, calcium salt crystalline Form I is characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 6.4°, 7.0°, 12.5°, 14.0°, 17.3°, 18.0°, and 23.3°. In another embodiment, calcium salt crystalline Form I is characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 6.4°, 7.0°, 12.5°, 14.0°, 17.3°, 18.0°, and 23.3°. In another embodiment, calcium salt crystalline Form I is characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 6.4°, 7.0°, 12.5°, 14.0°, 17.3°, 18.0°, and 23.3°. In another embodiment, calcium salt crystalline Form I is characterized by x-ray powder diffraction peaks at 2θ angles 6.4°, 7.0°, 12.5°, 14.0°, 17.3°, 18.0°, and 23.3°. In another embodiment, calcium salt crystalline Form I is characterized by at least three, four, five, six, or all x-ray powder diffraction peaks at 2θ angles selected from 6.4°, 7.0°, 12.5°, 14.0°, 17.3°, 18.0°, and 23.3°, and is further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 4.3°, 7.7°, 8.2°, 9.3°, 12.8°, 15.8°, 18.8°, 20.1°, and 21.1°. In another embodiment, calcium salt crystalline Form I is characterized by one or more, or all of the x-ray powder diffraction peaks at 2θ angles provided in Table 22A. In another embodiment, calcium salt crystalline Form I is characterized by an x-ray powder diffraction substantially similar to Figure 10A. In another embodiment, calcium salt crystalline Form I is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 10A, or the peaks recited in Table 22A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 73.1 °C, 135.8 °C and 200.2 °C ± 2 °C. 28 ME1\53438692.v1 136867-00920 In another embodiment, the molar ratio of calcium counter-ion to compound in calcium salt crystalline Form I is about 0.4, and calcium salt crystalline Form I is further characterized by the features in any one of the previous two paragraphs, Figure 10A, or the peaks recited in Table 22A. In another embodiment, calcium salt crystalline Form I is a hydrate, and is further characterized by the features in any one of the previous three paragraphs, Figure 10A, or the peaks recited in Table 22A. Calcium Salt Form II In one embodiment, calcium salt crystalline Form II is characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 4.3°, 8.3°, 8.6°, 13.0°, 14.0°, 15.9°, and 17.3°. In another embodiment, calcium salt crystalline Form II is characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 4.3°, 8.3°, 8.6°, 13.0°, 14.0°, 15.9°, and 17.3°. In another embodiment, calcium salt crystalline Form II is characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 4.3°, 8.3°, 8.6°, 13.0°, 14.0°, 15.9°, and 17.3°. In another embodiment, calcium salt crystalline Form II is characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 4.3°, 8.3°, 8.6°, 13.0°, 14.0°, 15.9°, and 17.3°. In another embodiment, calcium salt crystalline Form II is characterized by x-ray powder diffraction peaks at 2θ angles 4.3°, 8.3°, 8.6°, 13.0°, 14.0°, 15.9°, and 17.3°. In another embodiment, calcium salt crystalline Form II is characterized by at least three, four, five, six, or all x-ray powder diffraction peaks at 2θ angles selected from 4.3°, 8.3°, 8.6°, 13.0°, 14.0°, 15.9°, and 17.3°, and is further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 10.8°, 14.9°, 18.4°, and 23.2°. In another embodiment, calcium salt crystalline Form II is characterized by one or more, or all of the x-ray powder diffraction peaks at 2θ angles provided in Table 23A. In another embodiment, calcium salt crystalline Form II is characterized by an x-ray powder diffraction substantially similar to Figure 11A. In another embodiment, calcium salt crystalline Form II is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 11A, or the peaks recited in Table 23A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 93.0 °C and 253.9 °C ± 2 °C. In another embodiment, the molar ratio of calcium counter-ion to compound in calcium salt crystalline Form II is about 0.4, and calcium salt crystalline Form II is further 29 ME1\53438692.v1 136867-00920 characterized by the features in any one of the previous two paragraphs, Figure 11A, or the peaks recited in Table 23A. In another embodiment, calcium salt crystalline Form II is an anhydrate, and is further characterized by the features in any one of the previous three paragraphs, Figure 11A, or the peaks recited in Table 23A. Calcium Salt Form III In one embodiment, calcium salt crystalline Form III is characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 14.0°, 15.4°, 17.3°, 18.7°, 19.3°, 20.0°, and 22.8°. In another embodiment, calcium salt crystalline Form III is characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 14.0°, 15.4°, 17.3°, 18.7°, 19.3°, 20.0°, and 22.8°. In another embodiment, calcium salt crystalline Form III is characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 14.0°, 15.4°, 17.3°, 18.7°, 19.3°, 20.0°, and 22.8°. In another embodiment, calcium salt crystalline Form III is characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 14.0°, 15.4°, 17.3°, 18.7°, 19.3°, 20.0°, and 22.8°. In another embodiment, calcium salt crystalline Form III is characterized by x-ray powder diffraction peaks at 2θ angles 14.0°, 15.4°, 17.3°, 18.7°, 19.3°, 20.0°, and 22.8°. In another embodiment, calcium salt crystalline Form III is characterized by at least three, four, five, six, or all x-ray powder diffraction peaks at 2θ angles selected from 14.0°, 15.4°, 17.3°, 18.7°, 19.3°, 20.0°, and 22.8°, and is further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 12.6°, 13.3°, 20.5°, and 24.0°. In another embodiment, calcium salt crystalline Form III is characterized by one or more, or all of the x-ray powder diffraction peaks at 2θ angles provided in Table 24A. In another embodiment, calcium salt crystalline Form III is characterized by an x-ray powder diffraction substantially similar to Figure 12A. In another embodiment, calcium salt crystalline Form III is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 12A, or the peaks recited in Table 24A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising a peak endotherm at 216.0 °C ± 2 °C. In another embodiment, the molar ratio of calcium counter-ion to compound in calcium salt crystalline Form III is about 0.5, and calcium salt crystalline Form III is further characterized by the features in any one of the previous two paragraphs, Figure 12A, or the peaks recited in Table 24A. 30 ME1\53438692.v1 136867-00920 In another embodiment, calcium salt crystalline Form III is a DMSO solvate, and is further characterized by the features in any one of the previous three paragraphs, Figure 12A, or the peaks recited in Table 24A. Calcium Salt Form IV In one embodiment, calcium salt crystalline Form IV is characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 6.6°, 7.4°, 8.4°, 11.2°, 12.6°, 14.8°, 17.5°, 22.2°, and 23.3°. In another embodiment, calcium salt crystalline Form IV is characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 6.6°, 7.4°, 8.4°, 11.2°, 12.6°, 14.8°, 17.5°, 22.2°, and 23.3°. In another embodiment, calcium salt crystalline Form IV is characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 6.6°, 7.4°, 8.4°, 11.2°, 12.6°, 14.8°, 17.5°, 22.2°, and 23.3°. In another embodiment, calcium salt crystalline Form IV is characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 6.6°, 7.4°, 8.4°, 11.2°, 12.6°, 14.8°, 17.5°, 22.2°, and 23.3°. In another embodiment, calcium salt crystalline Form IV is characterized by at least seven x-ray powder diffraction peaks at 2θ angles selected from 6.6°, 7.4°, 8.4°, 11.2°, 12.6°, 14.8°, 17.5°, 22.2°, and 23.3°. In another embodiment, calcium salt crystalline Form IV is characterized by at least eight x-ray powder diffraction peaks at 2θ angles selected from 6.6°, 7.4°, 8.4°, 11.2°, 12.6°, 14.8°, 17.5°, 22.2°, and 23.3°. In another embodiment, calcium salt crystalline Form IV is characterized by x-ray powder diffraction peaks at 2θ angles 6.6°, 7.4°, 8.4°, 11.2°, 12.6°, 14.8°, 17.5°, 22.2°, and 23.3°. In another embodiment, calcium salt crystalline Form IV is characterized by at least three, four, five, six, seven, eight, or all x-ray powder diffraction peaks at 2θ angles selected from 6.6°, 7.4°, 8.4°, 11.2°, 12.6°, 14.8°, 17.5°, 22.2°, and 23.3°, and is further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 13.6°, 16.8°, 21.1°, and 35.2°. In another embodiment, calcium salt crystalline Form IV is characterized by one or more, or all of the x-ray powder diffraction peaks at 2θ angles provided in Table 25A. In another embodiment, calcium salt crystalline Form IV is characterized by an x-ray powder diffraction substantially similar to Figure 13A. In another embodiment, calcium salt crystalline Form IV is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 13A, or the peaks recited in Table 25A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 65.7 °C, 123.1 °C, 174.7 °C and 186.4 °C ± 2 °C. 31 ME1\53438692.v1 136867-00920 In another embodiment, the molar ratio of calcium counter-ion to compound in calcium salt crystalline Form IV is about 0.4, and calcium salt crystalline Form IV is further characterized by the features in any one of the previous two paragraphs, Figure 13A, or the peaks recited in Table 25A. Calcium Salt Form V In one embodiment, calcium salt crystalline Form V is characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 6.4°, 7.0°, 12.5°, 13.9°, 17.5°, 23.3°, 25.6°, 26.4°, and 26.9°. In another embodiment, calcium salt crystalline Form V is characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 6.4°, 7.0°, 12.5°, 13.9°, 17.5°, 23.3°, 25.6°, 26.4°, and 26.9°. In another embodiment, calcium salt crystalline Form V is characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 6.4°, 7.0°, 12.5°, 13.9°, 17.5°, 23.3°, 25.6°, 26.4°, and 26.9°. In another embodiment, calcium salt crystalline Form V is characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 6.4°, 7.0°, 12.5°, 13.9°, 17.5°, 23.3°, 25.6°, 26.4°, and 26.9°. In another embodiment, calcium salt crystalline Form V is characterized by at least seven x-ray powder diffraction peaks at 2θ angles selected from 6.4°, 7.0°, 12.5°, 13.9°, 17.5°, 23.3°, 25.6°, 26.4°, and 26.9°. In another embodiment, calcium salt crystalline Form V is characterized by at least eight x-ray powder diffraction peaks at 2θ angles selected from 6.4°, 7.0°, 12.5°, 13.9°, 17.5°, 23.3°, 25.6°, 26.4°, and 26.9°. In another embodiment, calcium salt crystalline Form V is characterized by x-ray powder diffraction peaks at 2θ angles 6.4°, 7.0°, 12.5°, 13.9°, 17.5°, 23.3°, 25.6°, 26.4°, and 26.9°. In another embodiment, calcium salt crystalline Form V is characterized by at least three, four, five, six, seven, eight, or all x-ray powder diffraction peaks at 2θ angles selected from 6.4°, 7.0°, 12.5°, 13.9°, 17.5°, 23.3°, 25.6°, 26.4°, and 26.9°, and is further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 7.7°, 9.3°, 15.4°, 21.1°, 22.2°, 24.6°, 28.8°, and 29.3°. In another embodiment, calcium salt crystalline Form V is characterized by one or more, or all of the x-ray powder diffraction peaks at 2θ angles provided in Table 25C. In another embodiment, calcium salt crystalline Form V is characterized by an x-ray powder diffraction substantially similar to Figure 14. In another embodiment, calcium salt crystalline Form V is a hydrate, and is further characterized any one of the sets of XRPD peaks of the previous paragraph, Figure 14, or the peaks recited in Table 25C. 32 ME1\53438692.v1 136867-00920 Choline Salt Form I In one embodiment, choline salt crystalline Form I is characterized by at least three x- ray powder diffraction peaks at 2θ angles selected from 11.2°, 12.8°, 14.1°, 16.7°, 17.1°, 20.4°, 21.4°, and 28.4°. In another embodiment, choline salt crystalline Form I is characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 11.2°, 12.8°, 14.1°, 16.7°, 17.1°, 20.4°, 21.4°, and 28.4°. In another embodiment, choline salt crystalline Form I is characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 11.2°, 12.8°, 14.1°, 16.7°, 17.1°, 20.4°, 21.4°, and 28.4°. In another embodiment, choline salt crystalline Form I is characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 11.2°, 12.8°, 14.1°, 16.7°, 17.1°, 20.4°, 21.4°, and 28.4°. In another embodiment, choline salt crystalline Form I is characterized by at least seven x-ray powder diffraction peaks at 2θ angles selected from 11.2°, 12.8°, 14.1°, 16.7°, 17.1°, 20.4°, 21.4°, and 28.4°. In another embodiment, choline salt crystalline Form I is characterized by x-ray powder diffraction peaks at 2θ angles 11.2°, 12.8°, 14.1°, 16.7°, 17.1°, 20.4°, 21.4°, and 28.4°. In another embodiment, choline salt crystalline Form I is characterized by at least three, four, five, six, seven, or all x-ray powder diffraction peaks at 2θ angles selected from 11.2°, 12.8°, 14.1°, 16.7°, 17.1°, 20.4°, 21.4°, and 28.4°, and is further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 16.4°, 18.9°, 22.5°, and 23.4°. In another embodiment, choline salt crystalline Form I is characterized by one or more, or all of the x-ray powder diffraction peaks at 2θ angles provided in Table 27A. In another embodiment, choline salt crystalline Form I is characterized by an x-ray powder diffraction substantially similar to Figure 15A. In another embodiment, choline salt crystalline Form I is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 15A, or the peaks recited in Table 27A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising a peak endotherm at 172.1 °C ± 2 °C. In another embodiment, the molar ratio of choline counter-ion to compound in choline salt crystalline Form I is about 1.0, and choline salt crystalline Form I is further characterized by the features in any one of the previous two paragraphs, Figure 15A, or the peaks recited in Table 27A. In another embodiment, choline salt crystalline Form I is an anhydrate, and is further characterized by the features in any one of the previous three paragraphs, Figure 15A, or the peaks recited in Table 27A. 33 ME1\53438692.v1 136867-00920 Choline Salt Form II In one embodiment, choline salt crystalline Form II is characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 6.6°, 9.9°, 10.9°, 13.3°, 20.0°, 21.4°, and 23.4°. In another embodiment, choline salt crystalline Form II is characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 6.6°, 9.9°, 10.9°, 13.3°, 20.0°, 21.4°, and 23.4°. In another embodiment, choline salt crystalline Form II is characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 6.6°, 9.9°, 10.9°, 13.3°, 20.0°, 21.4°, and 23.4°. In another embodiment, choline salt crystalline Form II is characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 6.6°, 9.9°, 10.9°, 13.3°, 20.0°, 21.4°, and 23.4°. In another embodiment, choline salt crystalline Form II is characterized by x-ray powder diffraction peaks at 2θ angles 6.6°, 9.9°, 10.9°, 13.3°, 20.0°, 21.4°, and 23.4°. In another embodiment, choline salt crystalline Form II is characterized by at least three, four, five, six, or all x-ray powder diffraction peaks at 2θ angles selected from 6.6°, 9.9°, 10.9°, 13.3°, 20.0°, 21.4°, and 23.4°, and is further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 11.7°, 21.8°, 23.4°, and 27.5°. In another embodiment, choline salt crystalline Form II is characterized by one or more, or all of the x-ray powder diffraction peaks at 2θ angles provided in Table 28. In another embodiment, choline salt crystalline Form II is characterized by an x-ray powder diffraction substantially similar to Figure 16. Choline Salt Form III In one embodiment, choline salt crystalline Form III is characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 7.4°, 11.1°, 14.8°, and 22.3°. In another embodiment, choline salt crystalline Form III is characterized by x-ray powder diffraction peaks at 2θ angles 7.4°, 11.1°, 14.8°, and 22.3°. In another embodiment, choline salt crystalline Form III is characterized by at least three, or all x-ray powder diffraction peaks at 2θ angles selected from 7.4°, 11.1°, 14.8°, and 22.3°, and is further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 16.5°, 18.6°, 20.3°, and 33.4°. In another embodiment, choline salt crystalline Form III is characterized by one or more, or all of the x-ray powder diffraction peaks at 2θ angles provided in Table 29A. In another embodiment, choline salt crystalline Form III is characterized by an x-ray powder diffraction substantially similar to Figure 17A. In another embodiment, choline salt crystalline Form III is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 17A, or the peaks recited in 34 ME1\53438692.v1 136867-00920 Table 29A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 131.8 °C, and 175.7 °C, and a peak exotherm at 135.3 °C ± 2 °C. In another embodiment, the molar ratio of choline counter-ion to compound in choline salt crystalline Form III is about 1.1, and choline salt crystalline Form III is further characterized by the features in any one of the previous two paragraphs, Figure 17A, or the peaks recited in Table 29A. In another embodiment, choline salt crystalline Form III is an anhydrate, and is further characterized by the features in any one of the previous three paragraphs, Figure 17A, or the peaks recited in Table 29A. Choline Salt Form IV In one embodiment, choline salt crystalline Form IV is characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 10.5°, 13.3°, 17.4°, 18.3°, 20.7°, and 23.8°. In another embodiment, choline salt crystalline Form IV is characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 10.5°, 13.3°, 17.4°, 18.3°, 20.7°, and 23.8°. In another embodiment, choline salt crystalline Form IV is characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 10.5°, 13.3°, 17.4°, 18.3°, 20.7°, and 23.8°. In another embodiment, choline salt crystalline Form IV is characterized by x-ray powder diffraction peaks at 2θ angles 10.5°, 13.3°, 17.4°, 18.3°, 20.7°, and 23.8°. In another embodiment, choline salt crystalline Form IV is characterized by at least three, four, five, or all x-ray powder diffraction peaks at 2θ angles selected from 10.5°, 13.3°, 17.4°, 18.3°, 20.7°, and 23.8°, and is further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 11.3°, 17.8°, 18.9°, 21.1°, 22.3°, 23.4°, and 24.3°. In another embodiment, choline salt crystalline Form IV is characterized by one or more, or all of the x-ray powder diffraction peaks at 2θ angles provided in Table 30A. In another embodiment, choline salt crystalline Form IV is characterized by an x-ray powder diffraction substantially similar to Figure 18A. In another embodiment, choline salt crystalline Form IV is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 18A, or the peaks recited in Table 30A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 116.4 °C, 142.3 °C, and 176.2 °C, and a peak exotherm at 144.6 °C ± 2 °C. 35 ME1\53438692.v1 136867-00920 In another embodiment, the molar ratio of choline counter-ion to compound in choline salt crystalline Form IV is about 1.1, and choline salt crystalline Form IV is further characterized by the features in any one of the previous two paragraphs, Figure 18A, or the peaks recited in Table 30A. In another embodiment, choline salt crystalline Form IV is an EtOH solvate, and is further characterized by the features in any one of the previous three paragraphs, Figure 18A, or the peaks recited in Table 30A. Choline Salt Form V In one embodiment, choline salt crystalline Form V is characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 10.6°, 14.5°, 17.4°, 18.6°, 20.7°, and 21.2°. In another embodiment, choline salt crystalline Form V is characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 10.6°, 14.5°, 17.4°, 18.6°, 20.7°, and 21.2°. In another embodiment, choline salt crystalline Form V is characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 10.6°, 14.5°, 17.4°, 18.6°, 20.7°, and 21.2°. In another embodiment, choline salt crystalline Form V is characterized by x-ray powder diffraction peaks at 2θ angles 10.6°, 14.5°, 17.4°, 18.6°, 20.7°, and 21.2°. In another embodiment, choline salt crystalline Form V is characterized by at least three, four, five, or all x-ray powder diffraction peaks at 2θ angles selected from 10.6°, 14.5°, 17.4°, 18.6°, 20.7°, and 21.2°, and is further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 11.4°, 15.6°, 17.8°, 19.8°, and 24.2°. In another embodiment, choline salt crystalline Form V is characterized by one or more, or all of the x- ray powder diffraction peaks at 2θ angles provided in Table 31A. In another embodiment, choline salt crystalline Form V is characterized by an x-ray powder diffraction substantially similar to Figure 19A. In another embodiment, choline salt crystalline Form V is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 19A, or the peaks recited in Table 31A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 142.2 °C, and 176.3 °C, and a peak exotherm at 144.8 °C ± 2 °C. In another embodiment, the molar ratio of choline counter-ion to compound in choline salt crystalline Form V is about 1.1, and choline salt crystalline Form V is further characterized by the features in any one of the previous two paragraphs, Figure 19A, or the peaks recited in Table 31A. 36 ME1\53438692.v1 136867-00920 In another embodiment, choline salt crystalline Form V is an anhydrate, and is further characterized by the features in any one of the previous three paragraphs, Figure 19A, or the peaks recited in Table 31A. Choline Salt Form VI In one embodiment, choline salt crystalline Form VI is characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 11.2°, 16.4°, 17.0°, 19.3°, 20.0°, 20.4°, and 22.9°. In another embodiment, choline salt crystalline Form VI is characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 11.2°, 16.4°, 17.0°, 19.3°, 20.0°, 20.4°, and 22.9°. In another embodiment, choline salt crystalline Form VI is characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 11.2°, 16.4°, 17.0°, 19.3°, 20.0°, 20.4°, and 22.9°. In another embodiment, choline salt crystalline Form VI is characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 11.2°, 16.4°, 17.0°, 19.3°, 20.0°, 20.4°, and 22.9°. In another embodiment, choline salt crystalline Form VI is characterized by x-ray powder diffraction peaks at 2θ angles 11.2°, 16.4°, 17.0°, 19.3°, 20.0°, 20.4°, and 22.9°. In another embodiment, choline salt crystalline Form VI is characterized by at least three, four, five, six, or all x-ray powder diffraction peaks at 2θ angles selected from 11.2°, 16.4°, 17.0°, 19.3°, 20.0°, 20.4°, and 22.9°, and is further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 11.2°, 16.4°, 17.0°, 19.3°, 20.0°, 20.4°. In another embodiment, choline salt crystalline Form VI is characterized by one or more, or all of the x-ray powder diffraction peaks at 2θ angles provided in Table 32A. In another embodiment, choline salt crystalline Form VI is characterized by an x-ray powder diffraction substantially similar to Figure 20A. In another embodiment, choline salt crystalline Form VI is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 20A, or the peaks recited in Table 32A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising a peak endotherm at 174.6 °C ± 2 °C. In another embodiment, the molar ratio of choline counter-ion to compound in choline salt crystalline Form VI is about 1.1, and choline salt crystalline Form VI is further characterized by the features in any one of the previous two paragraphs, Figure 20A, or the peaks recited in Table 32A. In another embodiment, choline salt crystalline Form VI is an anhydrate, and is further characterized by the features in any one of the previous three paragraphs, Figure 20A, or the peaks recited in Table 32A. 37 ME1\53438692.v1 136867-00920 HBr Salt Form I In one embodiment, hydrogen bromide salt crystalline Form I is characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 4.8°, 8.7°, 15.2°, 17.7°, 24.1°, and 30.0°. In another embodiment, hydrogen bromide salt crystalline Form I is characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 4.8°, 8.7°, 15.2°, 17.7°, 24.1°, and 30.0°. In another embodiment, hydrogen bromide salt crystalline Form I is characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 4.8°, 8.7°, 15.2°, 17.7°, 24.1°, and 30.0°. In another embodiment, hydrogen bromide salt crystalline Form I is characterized by x-ray powder diffraction peaks at 2θ angles 4.8°, 8.7°, 15.2°, 17.7°, 24.1°, and 30.0°. In another embodiment, hydrogen bromide salt crystalline Form I is characterized by at least three, four, five, or all x-ray powder diffraction peaks at 2θ angles selected from 4.8°, 8.7°, 15.2°, 17.7°, 24.1°, and 30.0°, and is further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 13.2°, 14.5°, 14.9°, and 15.8°. In another embodiment, hydrogen bromide salt crystalline Form I is characterized by one or more, or all of the x-ray powder diffraction peaks at 2θ angles provided in Table 34A. In another embodiment, hydrogen bromide salt crystalline Form I is characterized by an x-ray powder diffraction substantially similar to Figure 21A. In another embodiment, hydrogen bromide salt crystalline Form I is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 21A, or the peaks recited in Table 34A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 81.9 °C, 116.7 °C, 146.8 °C, and 169.7 °C ± 2 °C. In another embodiment, the molar ratio of bromide counter-ion to compound in hydrogen bromide salt crystalline Form I is about 0.7, and hydrogen bromide salt crystalline Form I is further characterized by the features in any one of the previous two paragraphs, Figure 21A, or the peaks recited in Table 34A. HBr Salt Form II In one embodiment, hydrogen bromide salt crystalline Form II is characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 4.9°, 10.8°, 14.5°, 15.3°, 19.4°, 23.6°, and 24.2°. In another embodiment, hydrogen bromide salt crystalline Form II is characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 4.9°, 10.8°, 14.5°, 15.3°, 19.4°, 23.6°, and 24.2°. In another embodiment, hydrogen bromide salt 38 ME1\53438692.v1 136867-00920 crystalline Form II is characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 4.9°, 10.8°, 14.5°, 15.3°, 19.4°, 23.6°, and 24.2°. In another embodiment, hydrogen bromide salt crystalline Form II is characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 4.9°, 10.8°, 14.5°, 15.3°, 19.4°, 23.6°, and 24.2°. In another embodiment, hydrogen bromide salt crystalline Form II is characterized by x-ray powder diffraction peaks at 2θ angles 4.9°, 10.8°, 14.5°, 15.3°, 19.4°, 23.6°, and 24.2°. In another embodiment, hydrogen bromide salt crystalline Form II is characterized by at least three, four, five, six, or all x-ray powder diffraction peaks at 2θ angles selected from 4.9°, 10.8°, 14.5°, 15.3°, 19.4°, 23.6°, and 24.2°, and is further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 6.8°, 9.7°, 15.6°, 17.4°, 21.6°, 29.2°, and 30.8°. In another embodiment, hydrogen bromide salt crystalline Form II is characterized by one or more, or all of the x-ray powder diffraction peaks at 2θ angles provided in Table 35A. In another embodiment, hydrogen bromide salt crystalline Form II is characterized by an x-ray powder diffraction substantially similar to Figure 22A. In another embodiment, hydrogen bromide salt crystalline Form II is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 22A, or the peaks recited in Table 35A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 111.2 °C and 147.8 °C ± 2 °C. In another embodiment, the molar ratio of bromide counter-ion to compound in hydrogen bromide salt crystalline Form II is about 1.0, and hydrogen bromide salt crystalline Form II is further characterized by the features in any one of the previous two paragraphs, Figure 22A, or the peaks recited in Table 35A. In another embodiment, hydrogen bromide salt crystalline Form II is a hydrate, and is further characterized by the features in any one of the previous three paragraphs, Figure 22A, or the peaks recited in Table 35A. HBr Salt Form III In one embodiment, hydrogen bromide salt crystalline Form III is characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 5.2°, 8.0°, 13.1°, 15.6°, 17.6°, 22.4°, and 28.9°. In another embodiment, hydrogen bromide salt crystalline Form III is characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 5.2°, 8.0°, 13.1°, 15.6°, 17.6°, 22.4°, and 28.9°. In another embodiment, hydrogen bromide salt crystalline Form III is characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 5.2°, 8.0°, 13.1°, 15.6°, 17.6°, 22.4°, and 28.9°. In another embodiment, 39 ME1\53438692.v1 136867-00920 hydrogen bromide salt crystalline Form III is characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 5.2°, 8.0°, 13.1°, 15.6°, 17.6°, 22.4°, and 28.9°. In another embodiment, hydrogen bromide salt crystalline Form III is characterized by x-ray powder diffraction peaks at 2θ angles 5.2°, 8.0°, 13.1°, 15.6°, 17.6°, 22.4°, and 28.9°. In another embodiment, hydrogen bromide salt crystalline Form III is characterized by at least three, four, five, six, or all x-ray powder diffraction peaks at 2θ angles selected from 5.2°, 8.0°, 13.1°, 15.6°, 17.6°, 22.4°, and 28.9°, and is further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 6.6°, 15.0°, 16.1°, 19.2°, 20.8°, and 21.1°. In another embodiment, hydrogen bromide salt crystalline Form III is characterized by one or more, or all of the x-ray powder diffraction peaks at 2θ angles provided in Table 36. In another embodiment, hydrogen bromide salt crystalline Form III is characterized by an x-ray powder diffraction substantially similar to Figure 23A. 1,5-Naphthalenedisulfonate Salt Form I In one embodiment, 1,5-naphthalenedisulfonate salt crystalline Form I is characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 8.3°, 11.1°, 12.2°, 14.0°, 15.7°, and 16.0°. In another embodiment, 1,5-naphthalenedisulfonate salt crystalline Form I is characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 8.3°, 11.1°, 12.2°, 14.0°, 15.7°, and 16.0°. In another embodiment, 1,5- naphthalenedisulfonate salt crystalline Form I is characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 8.3°, 11.1°, 12.2°, 14.0°, 15.7°, and 16.0°. In another embodiment, 1,5-naphthalenedisulfonate salt crystalline Form I is characterized by x- ray powder diffraction peaks at 2θ angles 8.3°, 11.1°, 12.2°, 14.0°, 15.7°, and 16.0°. In another embodiment, 1,5-naphthalenedisulfonate salt crystalline Form I is characterized by at least three, four, five, or all x-ray powder diffraction peaks at 2θ angles selected from 8.3°, 11.1°, 12.2°, 14.0°, 15.7°, and 16.0°, and is further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 7.5°, 13.1°, 14.5°, 15.0°, 16.4°, 16.7°, and 16.9°. In another embodiment, 1,5-naphthalenedisulfonate salt crystalline Form I is characterized by one or more, or all of the x-ray powder diffraction peaks at 2θ angles provided in Table 37A. In another embodiment, 1,5-naphthalenedisulfonate salt crystalline Form I is characterized by an x-ray powder diffraction substantially similar to Figure 24A. In another embodiment, 1,5-naphthalenedisulfonate salt crystalline Form I is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 24A, or the peaks recited in Table 37A, and is further characterized by a differential scanning 40 ME1\53438692.v1 136867-00920 calorimeter (DSC) thermogram comprising peak endotherms at 110.2 °C and 185.0 °C ± 2 °C. In another embodiment, the molar ratio of 1,5-naphthalenedisulfonate counter-ion to compound in 1,5-naphthalenedisulfonate salt crystalline Form I is about 0.7, and 1,5- naphthalenedisulfonate salt crystalline Form I is further characterized by the features in any one of the previous two paragraphs, Figure 24A, or the peaks recited in Table 37A. 1,5-Naphthalenedisulfonate Salt Form II In one embodiment, 1,5-naphthalenedisulfonate salt crystalline Form II is characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 5.9°, 13.2°, 18.2°, 18.6°, 23.2°, 25.8°, and 26.3°. In another embodiment, 1,5- naphthalenedisulfonate salt crystalline Form II is characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 5.9°, 13.2°, 18.2°, 18.6°, 23.2°, 25.8°, and 26.3°. In another embodiment, 1,5-naphthalenedisulfonate salt crystalline Form II is characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 5.9°, 13.2°, 18.2°, 18.6°, 23.2°, 25.8°, and 26.3°. In another embodiment, 1,5-naphthalenedisulfonate salt crystalline Form II is characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 5.9°, 13.2°, 18.2°, 18.6°, 23.2°, 25.8°, and 26.3°. In another embodiment, 1,5- naphthalenedisulfonate salt crystalline Form II is characterized by x-ray powder diffraction peaks at 2θ angles 5.9°, 13.2°, 18.2°, 18.6°, 23.2°, 25.8°, and 26.3°. In another embodiment, 1,5-naphthalenedisulfonate salt crystalline Form II is characterized by at least three, four, five, six, or all x-ray powder diffraction peaks at 2θ angles selected from 5.9°, 13.2°, 18.2°, 18.6°, 23.2°, 25.8°, and 26.3°, and is further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 7.5°, 14.1°, 15.7°, and 22.5°. In another embodiment, 1,5-naphthalenedisulfonate salt crystalline Form II is characterized by one or more, or all of the x-ray powder diffraction peaks at 2θ angles provided in Table 38A. In another embodiment, 1,5-naphthalenedisulfonate salt crystalline Form II is characterized by an x-ray powder diffraction substantially similar to Figure 25A. In another embodiment, 1,5-naphthalenedisulfonate salt crystalline Form II is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 25A, or the peaks recited in Table 38A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 130.9 ºC, 155.2 ºC and 164.3 ºC and a peak exotherm at 143.7 ºC ± 2 °C. 41 ME1\53438692.v1 136867-00920 In another embodiment, the molar ratio of 1,5-naphthalenedisulfonate counter-ion to compound in 1,5-naphthalenedisulfonate salt crystalline Form II is about 0.9, and 1,5- naphthalenedisulfonate salt crystalline Form II is further characterized by the features in any one of the previous two paragraphs, Figure 25A, or the peaks recited in Table 38A. Edisylate Salt Form I In one embodiment, edisylate salt crystalline Form I is characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 13.3°, 14.3°, 14.8°, and 19.1°. In another embodiment, edisylate salt crystalline Form I is characterized by x-ray powder diffraction peaks at 2θ angles 13.3°, 14.3°, 14.8°, and 19.1°. In another embodiment, edisylate salt crystalline Form I is characterized by at least three, or all x-ray powder diffraction peaks at 2θ angles selected from 13.3°, 14.3°, 14.8°, and 19.1°, and is further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 9.6°, 12.6°, 15.5°, and 17.3°. In another embodiment, edisylate salt crystalline Form I is characterized by one or more, or all of the x-ray powder diffraction peaks at 2θ angles provided in Table 39A. In another embodiment, edisylate salt crystalline Form I is characterized by an x-ray powder diffraction substantially similar to Figure 26A. In another embodiment, edisylate salt crystalline Form I is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 26A, or the peaks recited in Table 39A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 80.1 °C, 156.8 °C, and 170.5 °C ± 2 °C. In another embodiment, the molar ratio of edisylate counter-ion to compound in edisylate salt crystalline Form I is about 0.8, and edisylate salt crystalline Form I is further characterized by the features in any one of the previous two paragraphs, Figure 26A, or the peaks recited in Table 37A. Edisylate Salt Form II In one embodiment, edisylate salt crystalline Form II is characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 6.0°, 16.6°, 17.2°, 18.2°, 21.3°, 21.7°, and 22.4°. In another embodiment, edisylate salt crystalline Form II is characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 6.0°, 16.6°, 17.2°, 18.2°, 21.3°, 21.7°, and 22.4°. In another embodiment, edisylate salt crystalline Form II is characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 6.0°, 16.6°, 17.2°, 18.2°, 21.3°, 21.7°, and 22.4°. In another embodiment, edisylate salt crystalline Form II is characterized by at least six x-ray powder diffraction peaks at 2θ angles selected 42 ME1\53438692.v1 136867-00920 from 6.0°, 16.6°, 17.2°, 18.2°, 21.3°, 21.7°, and 22.4°. In another embodiment, edisylate salt crystalline Form II is characterized by x-ray powder diffraction peaks at 2θ angles 6.0°, 16.6°, 17.2°, 18.2°, 21.3°, 21.7°, and 22.4°. In another embodiment, edisylate salt crystalline Form II is characterized by at least three, four, five, six, or all x-ray powder diffraction peaks at 2θ angles selected from 6.0°, 16.6°, 17.2°, 18.2°, 21.3°, 21.7°, and 22.4°, and is further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 13.5°, 17.5°, 19.1°, and 23.0°. In another embodiment, edisylate salt crystalline Form II is characterized by one or more, or all of the x-ray powder diffraction peaks at 2θ angles provided in Table 40A. In another embodiment, edisylate salt crystalline Form II is characterized by an x-ray powder diffraction substantially similar to Figure 27A. In another embodiment, edisylate salt crystalline Form II is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 27A, or the peaks recited in Table 40A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 74.2 ºC, 116.5 ºC and 131.1 ºC and a peak exotherm at 143.7 ºC ± 2 °C. In another embodiment, the molar ratio of edisylate counter-ion to compound in edisylate salt crystalline Form II is about 0.8, and edisylate salt crystalline Form II is further characterized by the features in any one of the previous two paragraphs, Figure 27A, or the peaks recited in Table 40A. Diethylamine Salt Form I In one embodiment, diethylamine salt crystalline Form I is characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 12.9°, 13.4°, 17.7°, 19.0°, 21.4°, 25.0°, and 30.0°. In another embodiment, diethylamine salt crystalline Form I is characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 12.9°, 13.4°, 17.7°, 19.0°, 21.4°, 25.0°, and 30.0°. In another embodiment, diethylamine salt crystalline Form I is characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 12.9°, 13.4°, 17.7°, 19.0°, 21.4°, 25.0°, and 30.0°. In another embodiment, diethylamine salt crystalline Form I is characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 12.9°, 13.4°, 17.7°, 19.0°, 21.4°, 25.0°, and 30.0°. In another embodiment, diethylamine salt crystalline Form I is characterized by x-ray powder diffraction peaks at 2θ angles 12.9°, 13.4°, 17.7°, 19.0°, 21.4°, 25.0°, and 30.0°. In another embodiment, diethylamine salt crystalline Form I is characterized by at least three, four, five, six, or all x- ray powder diffraction peaks at 2θ angles selected from 12.9°, 13.4°, 17.7°, 19.0°, 21.4°, 43 ME1\53438692.v1 136867-00920 25.0°, and 30.0°, and is further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 8.7°, 13.2°, 14.9°, 15.1°, 15.8°, 17.0°, 20.3°, 21.1°, and 23.4°. In another embodiment, diethylamine salt crystalline Form I is characterized by one or more, or all of the x-ray powder diffraction peaks at 2θ angles provided in Table 41A. In another embodiment, diethylamine salt crystalline Form I is characterized by an x-ray powder diffraction substantially similar to Figure 28A. In another embodiment, diethylamine salt crystalline Form I is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 28A, or the peaks recited in Table 41A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 98.7 °C and 195.9 °C ± 2 °C. In another embodiment, the molar ratio of diethylamine counter-ion to compound in diethylamine salt crystalline Form I is about 0.5, and diethylamine salt crystalline Form I is further characterized by the features in any one of the previous two paragraphs, Figure 28A, or the peaks recited in Table 41A. Diethylamine Salt Form II In one embodiment, diethylamine salt crystalline Form II is characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 3.7°, 7.3°, 11.0°, 12.3°, 13.8°, 14.6°, 16.9°, and 17.9°. In another embodiment, diethylamine salt crystalline Form II is characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 3.7°, 7.3°, 11.0°, 12.3°, 13.8°, 14.6°, 16.9°, and 17.9°. In another embodiment, diethylamine salt crystalline Form II is characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 3.7°, 7.3°, 11.0°, 12.3°, 13.8°, 14.6°, 16.9°, and 17.9°. In another embodiment, diethylamine salt crystalline Form II is characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 3.7°, 7.3°, 11.0°, 12.3°, 13.8°, 14.6°, 16.9°, and 17.9°. In another embodiment, diethylamine salt crystalline Form II is characterized by at least seven x-ray powder diffraction peaks at 2θ angles selected from 3.7°, 7.3°, 11.0°, 12.3°, 13.8°, 14.6°, 16.9°, and 17.9°. In another embodiment, diethylamine salt crystalline Form II is characterized by x-ray powder diffraction peaks at 2θ angles 3.7°, 7.3°, 11.0°, 12.3°, 13.8°, 14.6°, 16.9°, and 17.9°. In another embodiment, diethylamine salt crystalline Form II is characterized by at least three, four, five, six, seven, or all x-ray powder diffraction peaks at 2θ angles selected from 3.7°, 7.3°, 11.0°, 12.3°, 13.8°, 14.6°, 16.9°, and 17.9°, and is further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 8.5°, 10.3°, 18.2°, 20.9°, and 22.9°. In another embodiment, diethylamine salt 44 ME1\53438692.v1 136867-00920 crystalline Form II is characterized by one or more, or all of the x-ray powder diffraction peaks at 2θ angles provided in Table 42A. In another embodiment, diethylamine salt crystalline Form II is characterized by an x-ray powder diffraction substantially similar to Figure 29A. In another embodiment, diethylamine salt crystalline Form II is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 29A, or the peaks recited in Table 42A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 119.8 ºC, 180.0 ºC and 192.0 ºC. In another embodiment, the molar ratio of diethylamine counter-ion to compound in diethylamine salt crystalline Form II is about 0.9, and diethylamine salt crystalline Form II is further characterized by the features in any one of the previous two paragraphs, Figure 29A, or the peaks recited in Table 42A. HCl Salt Form I In one embodiment, hydrogen chloride salt crystalline Form I is characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 4.8°, 6.8°, 14.4°, 15.3°, 19.4°, and 24.1°. In another embodiment, hydrogen chloride salt crystalline Form I is characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 4.8°, 6.8°, 14.4°, 15.3°, 19.4°, and 24.1°. In another embodiment, hydrogen chloride salt crystalline Form I is characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 4.8°, 6.8°, 14.4°, 15.3°, 19.4°, and 24.1°. In another embodiment, hydrogen chloride salt crystalline Form I is characterized by x-ray powder diffraction peaks at 2θ angles 4.8°, 6.8°, 14.4°, 15.3°, 19.4°, and 24.1°. In another embodiment, hydrogen chloride salt crystalline Form I is characterized by at least three, four, five, or all x-ray powder diffraction peaks at 2θ angles selected from 4.8°, 6.8°, 14.4°, 15.3°, 19.4°, and 24.1°, and is further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 9.7°, 15.9°, 21.7°, 29.2°, and 30.9°. In another embodiment, hydrogen chloride salt crystalline Form I is characterized by one or more, or all of the x-ray powder diffraction peaks at 2θ angles provided in Table 43A. In another embodiment, hydrogen chloride salt crystalline Form I is characterized by an x-ray powder diffraction substantially similar to Figure 30A. In another embodiment, hydrogen chloride salt crystalline Form I is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 30A, or the peaks recited in Table 43A, and is further characterized by a differential scanning calorimeter 45 ME1\53438692.v1 136867-00920 (DSC) thermogram comprising peak endotherms at 93.9 ºC, 137.6 ºC, 153.4 ºC, and 166.7 ºC ± 2 °C. In another embodiment, the molar ratio of chloride counter-ion to compound in hydrogen chloride salt crystalline Form I is about 0.6, and hydrogen chloride salt crystalline Form I is further characterized by the features in any one of the previous two paragraphs, Figure 30A, or the peaks recited in Table 43A. HCl Salt Form II In one embodiment, hydrogen chloride salt crystalline Form II is characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 4.8°, 8.7°, 13.3°, 17.8°, 24.1°, 29.0°, and 30.0°. In another embodiment, hydrogen chloride salt crystalline Form II is characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 4.8°, 8.7°, 13.3°, 17.8°, 24.1°, 29.0°, and 30.0°. In another embodiment, hydrogen chloride salt crystalline Form II is characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 4.8°, 8.7°, 13.3°, 17.8°, 24.1°, 29.0°, and 30.0°. In another embodiment, hydrogen chloride salt crystalline Form II is characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 4.8°, 8.7°, 13.3°, 17.8°, 24.1°, 29.0°, and 30.0°. In another embodiment, hydrogen chloride salt crystalline Form II is characterized by x-ray powder diffraction peaks at 2θ angles 4.8°, 8.7°, 13.3°, 17.8°, 24.1°, 29.0°, and 30.0°. In another embodiment, hydrogen chloride salt crystalline Form II is characterized by at least three, four, five, six, or all x-ray powder diffraction peaks at 2θ angles selected from 4.8°, 8.7°, 13.3°, 17.8°, 24.1°, 29.0°, and 30.0°, and is further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 5.4°, 9.6°, 12.4°, 14.4°, 19.2°, and 33.9°. In another embodiment, hydrogen chloride salt crystalline Form II is characterized by one or more, or all of the x-ray powder diffraction peaks at 2θ angles provided in Table 44. In another embodiment, hydrogen chloride salt crystalline Form II is characterized by an x-ray powder diffraction substantially similar to Figure 31. HCl Salt Form III In one embodiment, hydrogen chloride salt crystalline Form III is characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 4.8°, 6.3°, 8.7°, 14.2°, 16.5°, 23.5°, and 24.1°. In another embodiment, hydrogen chloride salt crystalline Form III is characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 4.8°, 6.3°, 8.7°, 14.2°, 16.5°, 23.5°, and 24.1°. In another embodiment, hydrogen chloride salt crystalline Form III is characterized by at least five x-ray powder diffraction peaks at 2θ 46 ME1\53438692.v1 136867-00920 angles selected from 4.8°, 6.3°, 8.7°, 14.2°, 16.5°, 23.5°, and 24.1°. In another embodiment, hydrogen chloride salt crystalline Form III is characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 4.8°, 6.3°, 8.7°, 14.2°, 16.5°, 23.5°, and 24.1°. In another embodiment, hydrogen chloride salt crystalline Form III is characterized by x-ray powder diffraction peaks at 2θ angles 4.8°, 6.3°, 8.7°, 14.2°, 16.5°, 23.5°, and 24.1°. In another embodiment, hydrogen chloride salt crystalline Form III is characterized by at least three, four, five, six, or all x-ray powder diffraction peaks at 2θ angles selected from 4.8°, 6.3°, 8.7°, 14.2°, 16.5°, 23.5°, and 24.1°, and is further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 8.1°, 19.2°, 20.3°, 25.1°, and 30.0°. In another embodiment, hydrogen chloride salt crystalline Form III is characterized by one or more, or all of the x-ray powder diffraction peaks at 2θ angles provided in Table 45. In another embodiment, hydrogen chloride salt crystalline Form III is characterized by an x-ray powder diffraction substantially similar to Figure 32. HCl Salt Form IV In one embodiment, hydrogen chloride salt crystalline Form IV is characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 4.8°, 8.7°, 13.2°, 13.3°, 15.8°, 17.7°, 21.1°, and 30.0°. In another embodiment, hydrogen chloride salt crystalline Form IV is characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 4.8°, 8.7°, 13.2°, 13.3°, 15.8°, 17.7°, 21.1°, and 30.0°. In another embodiment, hydrogen chloride salt crystalline Form IV is characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 4.8°, 8.7°, 13.2°, 13.3°, 15.8°, 17.7°, 21.1°, and 30.0°. In another embodiment, hydrogen chloride salt crystalline Form IV is characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 4.8°, 8.7°, 13.2°, 13.3°, 15.8°, 17.7°, 21.1°, and 30.0°. In another embodiment, hydrogen chloride salt crystalline Form IV is characterized by at least seven x-ray powder diffraction peaks at 2θ angles selected from 4.8°, 8.7°, 13.2°, 13.3°, 15.8°, 17.7°, 21.1°, and 30.0°. In another embodiment, hydrogen chloride salt crystalline Form IV is characterized by x-ray powder diffraction peaks at 2θ angles 4.8°, 8.7°, 13.2°, 13.3°, 15.8°, 17.7°, 21.1°, and 30.0°. In another embodiment, hydrogen chloride salt crystalline Form IV is characterized by at least three, four, five, six, seven, or all x-ray powder diffraction peaks at 2θ angles selected from 4.8°, 8.7°, 13.2°, 13.3°, 15.8°, 17.7°, 21.1°, and 30.0°, and is further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 5.4°, 14.2°, 14.9°, 16.2°, 17.4° and 19.6°. In another embodiment, hydrogen chloride salt crystalline Form IV is characterized by one or 47 ME1\53438692.v1 136867-00920 more, or all of the x-ray powder diffraction peaks at 2θ angles provided in Table 46A. In another embodiment, hydrogen chloride salt crystalline Form IV is characterized by an x-ray powder diffraction substantially similar to Figure 33A. In another embodiment, hydrogen chloride salt crystalline Form IV is characterized by any one of the sets of XRPD peaks of the previous paragraph, Figure 33A, or the peaks recited in Table 46A, and is further characterized by a differential scanning calorimeter (DSC) thermogram comprising a peak endotherm at 178.5 ºC, and peak exotherms at 91.6 ºC and 160.2 ºC. In another embodiment, the molar ratio of chloride counter-ion to compound in hydrogen chloride salt crystalline Form IV is about 0.3, and hydrogen chloride salt crystalline Form IV is further characterized by the features in any one of the previous two paragraphs, Figure 33A, or the peaks recited in Table 46A. Also provided herein are pharmaceutical compositions comprising any of one the crystalline salt Forms described herein. In one embodiment, the pharmaceutical composition comprises a pharmaceutically acceptable carrier and any of the crystalline salt Forms as described herein. In one embodiment, the pharmaceutical composition comprises at least one solid pharmaceutically acceptable carrier and any of the crystalline salt Forms as described herein. “Pharmaceutically acceptable carrier” refers to a substance that aids the formulation and/or administration of an active agent to and/or absorption by a subject and can be included in the compositions of the present disclosure without causing a significant adverse toxicological effect on the subject. Non-limiting examples of pharmaceutically acceptable carriers include water, NaCl, normal saline solutions, lactated Ringer’s, normal sucrose, normal glucose, binders, fillers, disintegrants, lubricants, coatings, sweeteners, flavors, salt solutions (such as Ringer’s solution), alcohols, oils, gelatins, carbohydrates such as lactose, amylose or starch, hydroxymethycellulose, fatty acid esters, polyvinyl pyrrolidine, and colors, and the like. Such preparations can be sterilized and, if desired, mixed with auxiliary agents such as lubricants, preservatives, stabilizers, wetting agents, emulsifiers, salts for influencing osmotic pressure, buffers, coloring, and/or aromatic substances and the like that do not deleteriously react with or interfere with the activity of the compounds provided herein. One of ordinary skill in the art will recognize that other pharmaceutical carriers are suitable for use with disclosed compounds. As used herein, a “solid pharmaceutically acceptable carrier” refers to carriers which are not in liquid form at room temperature. Thus, 48 ME1\53438692.v1 136867-00920 a “solid pharmaceutically acceptable carrier” excludes water and organic solvents such as acetonitrile. The pharmaceutical compositions described herein optionally include one or more pharmaceutically acceptable carriers such as lactose, starch, cellulose and dextrose. Other excipients, such as flavoring agents, sweeteners, and preservatives, such as methyl, ethyl, propyl and butyl parabens, can also be included. More complete listings of suitable excipients can be found in the Handbook of Pharmaceutical Excipients (5th Ed., Pharmaceutical Press (2005)). A person skilled in the art would know how to prepare formulations suitable for various types of administration routes. Conventional procedures and ingredients for the selection and preparation of suitable formulations are described, for example, in Remington's Pharmaceutical Sciences (2003 - 20th edition) and in The United States Pharmacopeia: The National Formulary (USP 24 NF19) published in 1999. The carriers, diluents and/or excipients are “acceptable” in the sense of being compatible with the other ingredients of the pharmaceutical composition and not deleterious to the recipient thereof. In one embodiment, provided are methods for inhibiting mitogen-activated protein kinase (MEK) or extra cellular signal-regulated kinases (ERK) in a subject in need thereof, comprising: administering to the subject an effective amount of any of the crystalline salt Forms described herein, or an effective amount of a pharmaceutical composition thereof. A “subject” is a mammal in need of treatment. The mammal can be a veterinary animal (e.g., dog or cat, and the like), farm animal (e.g., horse, cow, sheep or goat and the like) or laboratory animal (e.g., mouse, rat or guinea pig and the like). Most commonly, the subject is a human. A “subject in need of treatment” is a subject with a disease in which medical treatment is desirable. In some embodiments, the disease is cancer. In some embodiments, the cancer is selected from breast cancer, prostate cancer, esophageal cancer, colon cancer, endometrial cancer, blood cancer, brain cancer, glioma, head and neck cancer, thyroid cancer, gallbladder cancer, bladder cancer, skin cancer, malignant melanoma, cancer of the uterus, cancer of the ovary, lung cancer, pancreatic cancer, liver cancer, renal cancer, testicular cancer, renal pelvic and ureteral cancer, prostate cancer, gastric cancer, stomach cancer, and hematological cancer. In some embodiments, the lung cancer is selected from non-small cell lung cancer, small cell lung cancer, and lung carcinoid tumor. In some embodiments, the head and neck 49 ME1\53438692.v1 136867-00920 cancer is selected from pharyngeal cancer, laryngeal cancer, tongue cancer, and the like. In some embodiments, the hematological cancer is selected from leukemia, lymphoma, and multiple myeloma. In some embodiments, the hematological cancer is acute myeloblastic leukemia, chronic myeloid leukemia, B cell lymphoma, chronic lymphocytic leukemia (CLL), Non- Hodgkins lymphoma, hairy cell leukemia, Mantle cell lymphoma, Burkitt lymphoma, small lymphocytic lymphoma, follicular lymphoma, lymphoplasmacytic lymphoma, extranodal marginal zone lymphoma, activated B-cell like (ABC) diffuse large B cell lymphoma, or germinal center B cell (GCB) diffuse large B cell lymphoma. In some embodiments, the leukemia is selected from acute lymphoblastic leukemia (ALL), chronic lymphocytic leukemia (CLL), acute myelogenous leukemia (AML), acute myelocytic leukemia, acute lymphocytic leukemia, chronic myeloid leukemia (CML), chronic myelocytic leukemia, chronic lymphocytic leukemia, hairy cell leukemia, T-cell prolymphocytic leukemia, juvenile myelomonocytic leukemia, myelodysplastic syndrome, and follicular lymphoma. In some embodiments, the lymphoma is Hodgkin’s lymphoma or non-Hodgkin’s lymphoma (NHL). In some embodiments, the non-Hodgkin lymphoma (NHL) is selected from relapsed NHL, refractory NHL, and recurrent follicular NHL. In one embodiment, the cancer is characterized by an NRAS mutation. In another embodiment, the cancer is characterized by an NRAS mutation at position 61 (i.e., Q61X, where X is a naturally occurring amino acid). In another embodiment, the cancer is characterized by an NRAS Q61R, NRAS Q61L, NRAS Q61K, NRAS Q61P or NRAS Q61H mutation. In another embodiment, the cancer is characterized by an NRAS Q61R, NRAS Q61L, NRAS Q61K, NRAS Q61P or NRAS Q61H mutation and is a cancer of the bladder/urinary tract, lung, skin, liver, myeloid, lymphoid, ovarian/fallopian tube, peripheral nervous system, soft tissue or vulva/vagina. In another embodiment, the cancer is of the bladder/urinary tract, lung or skin, each characterized by an NRAS Q61R mutation; cancer of the liver, myeloid, skin, lymphoid or bladder/urinary tract, each characterized by an NRAS Q61L mutation; cancer of the lung, lymphoid, ovarian/fallopian tube, peripheral nervous system, soft tissue, vulva/vagina, liver or skin, each characterized by an NRAS Q61K mutation; cancer of the myeloid characterized by an NRAS Q61P mutation; or cancer of the soft tissue characterized by an NRAS Q61H mutation. In another embodiment, the cancer is 50 ME1\53438692.v1 136867-00920 characterized by an NRAS Q61R, NRAS Q61L, NRAS Q61K, NRAS Q61P or NRAS Q61H and is bladder urothelial carcinoma, non-small cell lung cancer, melanoma, hepatoblastoma, acute myeloid leukemia, non-hodgkin lymphoma, ovarian epithelial tumor, neuroblastoma, fibrosarcoma, mucosal melanoma of the vulva/vagina, hepatocellular carcinoma or rhabdomyosarcoma. In another embodiment, the cancer is characterized by an NRAS Q61R mutation, and is bladder urothelial carcinoma, non-small cell lung cancer or melanoma. In another embodiment, the cancer is characterized by an NRAS Q61L mutation, and is hepatoblastoma, acute myeloid leukemia, melanoma, non-hodgkin lymphoma or bladder urothelial carcinoma. In another embodiment, the cancer is characterized by an NRAS Q61K mutation, and is non-small cell lung cancer, non-hodgkin lymphoma, ovarian epithelial tumor, neuroblastoma, melanoma, fibrosarcoma, mucosal melanoma of the vulva/vagina or hepatocellular carcinoma. In another embodiment, the cancer is characterized by an NRAS Q61P mutation, and is acute myeloid leukemia. In another embodiment, the cancer is characterized by an NRAS Q61H mutation, and is rhabdomyosarcoma. In another embodiment, the cancer is characterized by an NRAS A91V or E132K mutation. In another embodiment, the cancer is characterized by an NRAS A91V or E132K mutation and is from the bowel, e.g., the cancer is colorectal adenocarcinoma. In another embodiment, the cancer is characterized by an NRAS T20 frame shift deletion. In another embodiment, the cancer is characterized by an NRAS T20 frame shift deletion and is from the lung, e.g., the cancer is lung neuroendocrine tumor. In another embodiment, the cancer is characterized by an NRAS G12C, G12V, G12D, G12A, G12S or G12R mutation. In another embodiment, the cancer is characterized by an NRAS G12C, G12V, G12D, G12A, G12S or G12R mutation and is a cancer from myeloid, skin, lymphoid or ovary/fallopian tubes. In another embodiment, the cancer is characterized by an NRAS G12C mutation and is from myeloid. In another embodiment, the cancer is characterized by an NRAS G12V mutation and is from skin. In another embodiment, the cancer is characterized by an NRAS G12D mutation and is from lymphoid, myeloid and ovaries/fallopian tubes. In another embodiment, the cancer is characterized by an NRAS G12R mutation and is from myeloid. In another embodiment, the cancer is characterized by an NRAS G12C, G12V, G12D, G12A, G12S or G12R mutation and is acute myeloid leukemia, non-hodgkins lymphoma, melanoma or ovarian epithelial tumor. In another embodiment, the cancer is characterized by an NRAS G12C mutation and is acute myeloid leukemia. In another embodiment, the cancer is characterized by an NRAS G12V mutation 51 ME1\53438692.v1 136867-00920 and is melanoma. In another embodiment, the cancer is characterized by an NRAS G12D mutation and is acute myeloid leukemia, non-hodgkins lympohoma or ovarian epithelial tumor. In another embodiment, the cancer is characterized by an NRAS G12R mutation and is acute myeloid leukemia. In another embodiment, the cancer is characterized by an NRAS G13D or NRAS G13R mutation. In another embodiment, the cancer is characterized by an NRAS G13D or NRAS G13R mutation and is a cancer of the myeloid, lymphoid or skin. In another embodiment, the cancer is characterized by an NRAS G13D mutation and is a cancer from lymphoid (e.g., non-hodgkin lymphoma). In another embodiment, the cancer is characterized by an NRAS G13R mutation and is a cancer from myeloid (e.g., acute myeloid leukemia) or skin (e.g., melanoma). In one embodiment, the cancer is characterized by a KRAS mutation. In another embodiment, the cancer is characterized by an KRAS mutation at position 13 (i.e., G13X, where X is a naturally occurring amino acid). In another embodiment, the cancer is characterized by a KRAS G13D, KRAS G13C or KRAS G13V mutation. In another embodiment, the cancer is characterized by a KRAS G13D, KRAS G13C or KRAS G13V mutation and is a cancer of the bowel, lung, breast. In another embodiment, the cancer is characterized by a KRAS G13D mutation and is of the bowel, lung or breast; or by a KRAS G13C mutation and is of the lung. In another embodiment, the cancer is characterized by a KRAS G13D or KRAS G13C mutation and is colorectal carcinoma, non-small lung cell cancer or invasive breast carcinoma. In another embodiment, the cancer is characterized by a KRAS mutation at V14L, V9I, I187V, A59T, P140H, A146T, L19F, A18D, A146V, K117N, P121H, A59G, V160A. In another embodiment, the cancer is lymphoid characterized by a KRAS mutation at V14L or V9I. In another embodiment, the cancer is bone characterized by a KRAS mutation at I187V or A59T. In another embodiment, the cancer is bowel characterized by a KRAS mutation at P140H or A146T. In another embodiment, the cancer is lung characterized by a KRAS mutation at L19F. In another embodiment, the cancer is myeloid characterized by a KRAS mutation at A18D, A146V or K117N. In another embodiment, the cancer is ovary/fallopian tube characterized by a KRAS mutation at P121H or A59G. In another embodiment, the cancer is uterus characterized by a KRAS mutation at V160A. In another embodiment, the cancer is characterized by a KRAS mutation at V14L and is B-lymphoblastic leukemia/lymphoma. In another embodiment, the cancer is characterized by a KRAS 52 ME1\53438692.v1 136867-00920 mutation at V9I and is non-hodgkin lymphoma. In another embodiment, the cancer is characterized by a KRAS mutation at I187V or A59T and is osteosarcoma. In another embodiment, the cancer is characterized by a KRAS mutation at P140H or A146T and is colorectal adenocarcinoma. In another embodiment, the cancer is characterized by a KRAS mutation at L19F and is non-small cell lung cancer. In another embodiment, the cancer is characterized by a KRAS mutation at A18D, A146V or K117N and is acute myeloid leukemia. In another embodiment, the cancer is characterized by a KRAS mutation at P121H or A59G and is ovarian epithelial tumor. In another embodiment, the cancer is characterized by a KRAS mutation at V160A and is endometrial carcinoma. In another embodiment, the cancer is characterized by an KRAS mutation at position 12 (i.e., G12X, where X is a naturally occurring amino acid). In another embodiment, the cancer is characterized by a KRAS G12D, G12V, G12A, G12R, G12S or G12C mutation. In another embodiment, the cancer is characterized by a KRAS G12D, G12V, G12A, G12R, G12S or G12C mutation and is a cancer of the bowel, esophagus/stomach, ovary/fallopian tube, pancreas, uterus, lung, soft tissue, biliary tract, breast, lymphoid, thyroid or cervix. In another embodiment, the cancer is characterized by a KRAS G12D mutation and is a cancer of the bowel, esophagus/stomach, ovary/fallopian tube, pancreas, uterus or lung, In another embodiment, the cancer is characterized by a KRAS G12V mutation and is a cancer of the bowel, lung, pancreas, uterus, soft tissue, biliary tract or breast. In another embodiment, the cancer is characterized by a KRAS G12A mutation and is a cancer of the lymphoid, lung or bowel. In another embodiment, the cancer is characterized by a KRAS G12R mutation and is a cancer of the thyroid or pancreas. In another embodiment, the cancer is characterized by a KRAS G12S mutation and is a cancer of the lungs or bowel. In another embodiment, the cancer is characterized by a KRAS G12C mutation and is a cancer of the bowel, lung, cervix, esophagus/stomach or pancreas. In another embodiment, the cancer is characterized by a KRAS G12D, G12V, G12A, G12R, G12S or G12C mutation and is colorectal adenocarcinoma, esophagogastric adenocarcinoma, ovarian epithelial tumor, pancreatic adenocarcinoma, endometrial carcinoma, non-small cell lung cancer, lung neuroendocrine tumor, leiomyosarcoma, intraductal papillary neoplasm of the bile duct, invasive breast carcinoma, non-hodgkin lymphoma, anaplastic thyroid cancer, cervical squamous cell carcinoma or esophageal squamous cell carcinoma. In another embodiment, the cancer is characterized by a KRAS G12D and is colorectal adenocarcinoma, esophagogastric adenocarcinoma, ovarian epithelial 53 ME1\53438692.v1 136867-00920 tumor, pancreatic adenocarcinoma, endometrial carcinoma or non-small cell lung cancer. In another embodiment, the cancer is characterized by a KRAS G12V mutation and is colorectal adenocarcinoma, non-small cell lung cancer, lung neuroendocrine tumor, pancreatic adenocarcinoma, endometrial carcinoma, leiomyosarcoma, intraductal papillary neoplasm of the bile duct or invasive breast carcinoma. In another embodiment, the cancer is characterized by a KRAS G12A mutation and is colorectal adenocarcinoma, non-hodgkin lymphoma or non-small cell lung cancer. In another embodiment, the cancer is characterized by a KRAS G12R mutation and is anaplastic thyroid cancer or pancreatic adenocarcinoma. In another embodiment, the cancer is characterized by a KRAS G12S mutation and is non-small cell lung cancer or colorectal adenocarincoma. In another embodiment, the cancer is characterized by an KRAS mutation at position 61 (i.e., Q61X, where X is a naturally occurring amino acid). In another embodiment, the cancer is characterized by a KRAS Q61H, Q61L, Q61K, Q61R, Q61P or G61E mutation. In another embodiment, the cancer is characterized by a KRAS Q61H, Q61L, Q61K, Q61R, Q61P or Q61E mutation and are cancers of the bowel, pancreas or lung. In another embodiment, the cancer is characterized by a Q61H KRAS mutation and is a cancer of the bowel or pancreas. In another embodiment, the cancer is characterized by a KRAS Q61L mutation and is a cancer of the bowel. In another embodiment, the cancer is characterized by a KRAS Q61K and is a cancer of the lung. In another embodiment, the cancer is characterized by a KRAS Q61R and is a cancer of the lung. In another embodiment, the cancer is characterized by a KRAS Q61H, Q61L, Q61K, Q61R, Q61P or G61E mutation and is colorectal adenocarcinoma, pancreatic adenocarcinoma or non-small cell lung cancer. In another embodiment, the cancer is characterized by a KRAS Q61R and is non-small cell lung cancer. In another embodiment, the cancer is characterized by a KRAS Q61H mutation and is colorectal adenocarcinoma or pancreatic adenocarcinoma. In another embodiment, the cancer is characterized by a KRAS Q61L mutation and is colorectal adenocarcinoma. In another embodiment, the cancer is characterized by a KRAS Q61K mutation and is non-small cell lung cancer. A subject with one of the aforementioned cancers may be treated by administering to the subject an effective amount of any one of crystalline salt Forms as described herein, or a pharmaceutical composition thereof. In some embodiments, the methods comprise administering an effective amount of a any one of crystalline salt Forms as described herein, or a pharmaceutical composition 54 ME1\53438692.v1 136867-00920 thereof, in combination with an effective amount of an anticancer agent, wherein the amounts of the combination and the chemotherapeutic are together effective in treating a subject with cancer. Many chemotherapeutics are presently known in the art and can be used in combination. In some embodiments, the chemotherapeutic is selected from mitotic inhibitors, alkylating agents, anti-metabolites, intercalating antibiotics, growth factor inhibitors, cell cycle inhibitors, enzymes, topoisomerase inhibitors, biological response modifiers, anti- hormones, angiogenesis inhibitors, and anti- androgens. Also described are methods for treating a subject with cancer comprising administering to the mammal an amount of a MEK protein kinase inhibitor and/or Raf protein kinase inhibitor in combination with radiation therapy, wherein the amounts of the MEK protein kinase inhibitor and/or Raf protein kinase inhibitor in combination with the radiation therapy effective in treating a subject with cancer. Techniques for administering radiation therapy are known in the art, and these techniques can be used in the combination therapy described herein. In some embodiments, the disclosure also relates to a method of inhibiting abnormal cell growth in a mammal which may comprise any one of crystalline salt Forms as described herein, or a pharmaceutical composition thereof, and an amount of one or more substances selected from anti-angiogenesis agents, signal transduction inhibitors, and antiproliferative agents. Anti-angiogenesis agents, such as MMP-2 (matrix-metalloprotienase 2) inhibitors, MMP-9 (matrix-metalloprotienase 9) inhibitors, and COX- 11 (cyclooxygenase 11) inhibitors, can be used in conjunction with a compound of the present invention and pharmaceutical compositions described herein. Examples of useful COX-II inhibitors include CELEBREXTM (alecoxib), valdecoxib, and rofecoxib. Examples of useful matrix metalloproteinase inhibitors are described in WO 96/33172 (published October 24,1996), WO 96/27583 (published March 7,1996), European Patent Application No.97304971.1 (filed luly 8,1997), European Patent Application No. 99308617.2 (filed October 29, 1999), WO 98/07697 (published February 26,1998), WO 98/03516 (published January 29.1998), WO 98/34918 (published August 13,1998), WO 98/34915 (published August 13.1998), WO 98/33768 (published August 6,1998), WO 98/30566 (published July 16, 1998), European Patent Publication 606,046 (published July 13,1994), European Patent Publication 931, 788 (published July 28,1999), WO 90/05719 (published May 31,1990), WO 99/52910 (published October 21,1999), WO 99/52889 (published October 21, 1999), WO 99/29667 (published June 17,1999), PCT International Application No. PCT/IB98/01113 (filed July 21,19911), European Patent Application No. 99302232.1 (filed March 25,1999), Great Britain Patent 55 ME1\53438692.v1 136867-00920 Application No. 9912961.1 (filed June 3, 1999), United States Provisional Application No. 60/148,464 (filed August 12,1999), United States Patent 5,863, 949 (issued January 26,1999), United States Patent 5,861, 510 (issued January 19,1999), and European Patent Publication 780,386 (published June 25, 1997). Some MMP-2 and MMP-9 inhibitors have little or no activity inhibiting MMP-1, while some selectively inhibit MMP-2 and/or AMP-9 relative to the other matrix-metalloproteinases (L e., MAP-1, NEMP-3, MMP-4, M7vlP-5, MMP-6, MMP- 7, MMP-8, MMP-10, MMP-11, and MMP-13). Some specific examples of MlvlP inhibitors useful in the present invention are AG-3340, RU 32-3555, and RS 13-0830. In some embodiments, any one of the crystalline salt Forms as described herein, or a pharmaceutical composition thereof, is administered with at least one additional therapeutic agent. In some embodiments, the therapeutic agent is a taxol, bortezornib or both. In further or additional embodiments, the therapeutic agent is selected from cytotoxic agents, anti- angiogenesis agents and antineoplastic agents. In further or additional embodiments, the anti- neoplastic agents selected from the group of consisting of alkylating agents, anti-metabolites, epiclophyllotoxims; antineoplastic enzymes, topoisomerase inhibitors, procarbazine, mitoxantrone, platinum coordination complexes, biological response modifiers and growth inhibitors, hormonal/anti-hormonal therapeutic agents, and haematopoietic growth factors. Many chemotherapeutics are presently known in the art and can be used in combination with any one of the crystalline salt Forms as described herein, or a pharmaceutical composition thereof. In some embodiments, the chemotherapeutic is selected from mitotic inhibitors, alkylating agents, anti-metabolites, intercalating antibiotics, growth factor inhibitors, cell cycle inhibitors, enzymes, topoisomerase inhibitors, biological response modifiers, anti-hormones, angiogenesis inhibitors, and anti-androgens. In some embodiments, the combination is administered in combination with an additional therapy. In further or additional embodiments, the additional therapy is radiation therapy, chemotherapy, surgery or any combination thereof. In further or additional embodiments, the combination is administered in combination with at least one additional therapeutic agent. In further or additional embodiments, the therapeutic agent is selected from the group of cytotoxic agents, anti-angiogenesis agents and antineoplastic agents. In further or additional embodiments, the anti-neoplastic agent is selected from of alkylating agents, anti-metabolites, epidophyllotoxins; antineoplastic enzymes, topoisomerase inhibitors, procarbazines, mitoxantrones, platinum coordination complexes, biological response 56 ME1\53438692.v1 136867-00920 modifiers and growth inhibitors, hormonal/anti-hormonal therapeutic agents, and haematopoietic growth factors. In some embodiments, the second therapeutic is an agent for co-regulating MEK or RAF pathways. In some embodiments, the second therapeutic agent is a MEK or RAF inhibitor. In some embodiments, the RAF inhibitor is vemurafenib, dabrafenlb, XL-281, LGX-818, CEP-32496. ARQ-736, MEK-162, refametinib, E-620L pimasertib, WX-554, GDC-0973 or LXH254. In some embodiments, the second therapeutic is an agent for co-regulating MAPK pathway. In some embodiments, the agent for co-regulating MAPK pathway is KRAS G12C mutant selective inhibitors including but not limited to sotorasib, adagrasib, ARS-1620, ARS- 3248, LY3499446, AMG-510, and MRTX849; KRAS G12D mutant selective inhibitors; Son of Sevenless 1 (SOS1) inhibitors (e.g., BI1701963, BI-3406 and RMC-023); SHP2 inhibitors (e.g, TNO155, BBP-398 and ICP-189) ; EGFR inhibitors including but not limited to gefitinib, erlotinib, afatinib, lazertinib, aumolertinib (formerly almonertinib), olmutinib, dacomitinib, nazartinib and osimertinib. In some embodiments, the second therapeutic is an agent for mutant p53 reactivators (PC14586, APR-246 and COTI-2). In some embodiments, the second therapeutic agent is selected from aspirin; diflunisal; salsalate; acetaminophen; ibuprofen; dexibuprofen; naproxen; fenoprofen; ketoprofen; dexketoprofen; flurbiprofen; oxaprozin; loxoprofen; indomethacin; tolmetin; sulindac; etodolac; ketorolac; diclofenac; aceclofenac; nabumetone; enolic acid; piroxicam; meloxicam; tenoxicam; droxicam; lomoxicam; isoxicam; mefenamic acid; meclofenamic acid; flufenamic acid; tolfenamic acid; sulfonanilides; clonixin; licofelone; dexamethasone; and prednisone. In some embodiments, the second therapeutic agent is selected from mechlorethamine; cyclophosphamide; melphalan; chlorambucil; ifosfamide; busulfan; N- nitroso-N-methylurea (MNU); carmustine (BCNU); lomustine (CCNU); semustine (MeCCNU); fotemustine; streptozotocin; dacarbazine; mitozolomide; temozolomide; thiotepa; mytomycin; diaziquone (AZQ); cisplatin; carboplatin; and oxaliplatin. In some embodiments, the second therapeutic agent is selected from vincristine; vinblastine; vinorelbine; vindesine; vinflunine; paclitaxel; docetaxel; etoposide; teniposide; tofacitinib; ixabepilone; irinotecan; topotecan; camptothecin; doxorubicin; mitoxantrone; and teniposide. 57 ME1\53438692.v1 136867-00920 In some embodiments, the second therapeutic agent is selected from actinomycin; bleomycin; plicamycin; mitomycin; daunombicin; epimbicin; idarubicin; pirarubicin; aclarubicin; mitoxantrone; cyclophosphamide; methotrexate; 5-fluorouracil; prednisolone; folinic acid; methotrexate; melphalan; capecitabine; mechlorethamine; uramustine; melphalan; chlorambucil; ifosfamide; bendamustine; 6-mercaptopurine; and procarbazine. In some embodiments, the second therapeutic agent is selected from cladribine; pemetrexed; fludarabine; gemcitabine; hydroxyurea; nelarabine; cladribine; clofarabine; ytarabine; decitabine; cytarabine; cytarabine liposomal; pralatrexate; floxuridine; fludarabine; colchicine; thioguanine; cabazitaxel; larotaxel; ortataxel; tesetaxel; aminopterin; pemetrexed; pralatrexate; raltitrexed; pemetrexed; carmofur; and floxuridine. In some embodiments, the second therapeutic agent is selected from azacitidine; decitabine; hydroxycarbamide; topotecan; irinotecan; belotecan; teniposide; aclarubicin; epimbicin; idarubicin; amrubicin; pirarubicin; valrubicin; zombicin; mitoxantrone; pixantrone; mechlorethamine; chlorambucil; prednimu stine; uramustine; estramustine; carmustine; lomustine; fotemustine; nimustine; ranimustine; carboquone; thioTEPA; triaziquone; and triethylenemelamine. In some embodiments, the second therapeutic agent is selected from nedaplatin; satraplatin; procarbazine; dacarbazine; temozolomide; altretamine; mitobronitol; pipobroman; actinomycin; bleomycin; plicamycin; aminolevulinic acid; methyl aminolevulinate; efaproxiral; talaporfin; temoporfin; verteporfin; alvocidib; seliciclib; palbociclib; bortezomib; carfilzomib; anagrelide; masoprocol; olaparib; belinostat; panobinostat; romidepsin; vorinosta; idelalisib; atrasentan; bexarotene; testolactone; amsacrine; trabectedin; alitretinoin; tretinoin; demecolcine; elsamitrucin; etoglucid; lonidamine; lucanthone; mitoguazone; mitotane; oblimersen; omacetaxine mepesuccinate; and eribulin. In some embodiments, the second therapeutic agent is selected from azathioprine; Mycophenolic acid; leflunomide; teriflunomide; tacrolimus; cyclosporin; pimecrolimus; abetimus; gusperimus; lenalidomide; pomalidomide; thalidomide; anakinra; sirolimus; everolimus; ridaforolimus; temsirolimus; umirolimus; zotarolimus; eculizumab; adalimumab; afelimomab; certolizumab pegol; golimumab; infliximab; nerelimomab; mepolizumab; omalizumab; faralimomab; elsilimomab; lebrikizumab; ustekinumab; etanercept; otelixizumab; teplizumab; visilizumab; clenoliximab; keliximab; zanolimumab; efalizumab; erlizumab; obinutuzumab; rituximab; and ocrelizumab. 58 ME1\53438692.v1 136867-00920 In some embodiments, the second therapeutic agent is selected from pascolizumab; gomiliximab; lumiliximab; teneliximab; toralizumab; aselizumab; galiximab; gavilimomab; ruplizumab; belimumab; blisibimod; ipilimumab; tremelimumab; bertilimumab; lerdelimumab; metelimumab; natalizumab; tocilizumab; odulimomab; basiliximab; daclizumab; inolimomab; zolimoma; atorolimumab; cedelizumab; fontolizumab; maslimomab; morolimumab; pexelizumab; reslizumab; rovelizumab; siplizumab; talizumab; telimomab; vapaliximab; vepalimomab; abatacept; belatacept; pegsunercept; aflibercept; alefacept; and rilonacept. In some embodiments, the second therapeutics is an immune checkpoint inhibitor such as a PD-1 inhibitor or a PD-L1 inhibitor. In some embodiments, the immune checkpoint inhibitor is an anti PD-1 antibody selected from balstilimab, camrelizumab, cemiplimab, dostarlimab, geptanolimab, nivolumab, pembrolizumab, penpulimab, pidilizumab, prolgolimab, retifanlimab, sasanlimab, serplulimab, serplulimab, sintilimab, spartalizumab, sulituzumab, tebotelimab, teripalimab, tislelizumab, toripalimab, toripalimab, zimberelimab, AMP -224 (Medlmunne), AMP-514 (Medlmunne), AT-16201 (AIMM Therapeutics BV), AVI-102 (Ab Vision Inc), BAT-1308 (Bio-Thera Solutions Ltd), BH-2950 (Beijing Hanmi Pharmaceutical Co Ltd), BSI-050K01 (Biosion Inc), CB-201 (Crescendo Biologies Ltd), CYTO-101 (Cytocom Inc), DB-004 (DotBio Pte Ltd), EX- 105 (Excelmab Inc), EX- 108 (Excelmab Inc), GNR-051 (Generium), HAB-21 (Suzhou Stainwei Biotech Inc), IBI-319 (Innovent Biologies Inc), IBI-321 (Innovent Biologies Inc), IKT-202 (Icell Kealex Therapeutics LLC), IMU-201 (Imugene Ltd), JS-201 (Shanghai Junshi Bioscience Co Ltd), LBL-006 (Leads Biolabs Inc), LBL-024 (Leads Biolabs Inc), LD-01 (Leidos Health Holdings LLC), LQ-005 (Shanghai Novamab Biopharmaceuticals Co Ltd), LQ-008 (Shanghai Novamab Biopharmaceuticals Co Ltd), MD-402 (MD Biosciences GmbH), OT-2 (OncoTrap Inc), PE-0105 (Shanghai Yunyi Health Technology Development Co Ltd), PF-07209960 (Pfizer Inc), PH-762 (Phio Pharmaceuticals Corp), REGN-PD-l/XX (Regeneron), R07121661 (Genentech), SAUG-1 (Juvenescence UK Ltd), SCT-IIOA (Sinocelltech), SG-001 (CSPC Pharmaceutical Group Ltd), SI-B003 (Systlmmune), SL-279137 (Shattuck Labs), SSI-361 (Lyvgen Biopharma Ltd), STI-A1110 (Servier), STM-418 (Stcube Inc), Sym-021 (Symphogen A/S), TSR-075 (GlaxoSmithKline Pic), TY101 (Tayu Huaxia Biotech), Twist- PD-1 (Twist Bioscience), XmAb-TGFpR2 (Xencor), XmAb-YYCD28 (Xencor), XmAb20717 (Xencor), XmAb23104 (Xencor), YBL-006 (Y Biologies), YBL-019 (Y Biologies), and mDX-400 (Merck & Co Inc). 59 ME1\53438692.v1 136867-00920 In one embodiment, the anti-cancer agent and any one of the crystalline salt Forms as described herein, or a pharmaceutical composition thereof, are administered contemporaneously. When administered contemporaneously, the anti-cancer agent and any one of the crystalline salt Forms can be administered in the same formulation or in different formulations. Alternatively, any one of the crystalline salt Forms as described herein and the additional anti-cancer agent are administered separately. Alternatively, any one of the crystalline salt Forms as described herein, and the additional anti-cancer agent can be administered sequentially, as separate compositions, within an appropriate time frame (e.g., a cancer treatment session/interval (e.g., about 1.5 to about 5 hours to about 10 hours to about 15 hours to about 20 hours; about 1 day to about 2 days to about 5 days to about 10 days to about 14 days)) as determined by the skilled clinician (e.g., a time sufficient to allow an overlap of the pharmaceutical effects of the therapies). Any one of the crystalline salt Forms as described herein and the additional anti-cancer agent can be administered in a single dose or multiple doses in an order and on a schedule suitable to achieve a desired therapeutic effect (e.g., inhibition of tumor growth). As used herein, the term "treating" or “treatment" refers to obtaining a desired pharmacological and/or physiological effect. The effect can be therapeutic, which includes achieving, partially or substantially, one or more of the following results: partially or totally reducing the extent of the disease, disorder or syndrome; ameliorating or improving a clinical symptom or indicator associated with the disorder; or delaying, inhibiting or decreasing the likelihood of the progression of the disease, disorder or syndrome. The precise amount of any one of the crystalline salt Forms as described herein administered to provide an “effective amount” to the subject will depend on the mode of administration, the type, and severity of the disease or condition, and on the characteristics of the subject, such as general health, age, sex, body weight, and tolerance to drugs. The skilled artisan will be able to determine appropriate dosages depending on these and other factors. When administered in combination with other therapeutic agents, e.g., when administered in combination with an anti-cancer agent, an “effective amount” of any additional therapeutic agent(s) will depend on the type of drug used. Suitable dosages are known for approved therapeutic agents and can be adjusted by the skilled artisan according to the condition of the subject, the type of condition(s) being treated and the amount of a compound of the invention being used by following, for example, dosages reported in the literature and recommended in the Physician’s Desk Reference (57th Ed., 2003). 60 ME1\53438692.v1 136867-00920 The term “effective amount” means an amount when administered to the subject which results in beneficial or desired results, including clinical results, e.g., inhibits, suppresses or reduces the symptoms of the condition being treated in the subject as compared to a control. For example, a therapeutically effective amount can be given in unit dosage form (e.g., 0.1 mg to about 50 g per day). The terms “administer”, “administering”, “administration”, and the like, as used herein, refer to methods that may be used to enable delivery of compositions to the desired site of biological action. These methods include, but are not limited to, intraarticular (in the joints), intravenous, intramuscular, intratumoral, intradermal, intraperitoneal, subcutaneous, orally, topically, intrathecally, inhalationally, transdermally, rectally, and the like. Administration techniques that can be employed with the agents and methods described herein are found in e.g., Goodman and Gilman, The Pharmacological Basis of Therapeutics, current ed.; Pergamon; and Remington’s, Pharmaceutical Sciences (current edition), Mack Publishing Co., Easton, Pa. The particular mode of administration and the dosage regimen will be selected by the attending clinician, taking into account the particulars of the case (e.g. the subject, the disease, the disease state involved, the particular treatment). Treatment can involve daily or multi-daily or less than daily (such as weekly or monthly etc.) doses over a period of a few days to months, or even years. However, a person of ordinary skill in the art would immediately recognize appropriate and/or equivalent doses looking at dosages of approved compositions for treating a disease using the disclosed MEK inhibitors for guidance. Any one of the crystalline salt Forms as described herein, or a pharmaceutical composition thereof, can be administered to a patient in a variety of forms depending on the selected route of administration, as will be understood by those skilled in the art. The compounds of the present teachings may be administered, for example, by oral, parenteral, buccal, sublingual, nasal, rectal, patch, pump or transdermal administration and the pharmaceutical compositions formulated accordingly. Parenteral administration includes intravenous, intraperitoneal, subcutaneous, intramuscular, transepithelial, nasal, intrapulmonary, intrathecal, rectal and topical modes of administration. Parenteral administration can be by continuous infusion over a selected period of time. The pharmaceutical composition described herein is formulated to be compatible with its intended route of administration. In an embodiment, the composition is formulated in accordance with routine procedures as a pharmaceutical composition adapted for intravenous, 61 ME1\53438692.v1 136867-00920 subcutaneous, intramuscular, oral, intranasal, or topical administration to human beings. In preferred embodiments, the pharmaceutical composition is formulated for intravenous administration. Typically, for oral therapeutic administration, a compound of the present teachings may be incorporated with excipient and used in the form of ingestible tablets, buccal tablets, troches, capsules, elixirs, suspensions, syrups, wafers, and the like. Typically for parenteral administration, solutions of a compound of the present teachings can generally be prepared in water suitably mixed with a surfactant such as hydroxypropylcellulose. Dispersions can also be prepared in glycerol, liquid polyethylene glycols, DMSO and mixtures thereof with or without alcohol, and in oils. Under ordinary conditions of storage and use, these preparations contain a preservative to prevent the growth of microorganisms. Typically, for injectable use, sterile aqueous solutions or dispersion of, and sterile powders of, a compound described herein for the extemporaneous preparation of sterile injectable solutions or dispersions are appropriate. The following Examples are offered to illustrate exemplary embodiments of the invention and do not define nor limit its scope. EXEMPLIFICATION Preparation of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3- fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one) Compound 1 can be prepared following the procedures for Example 35 in PCT/US2023/019588, reproduced below. To a solution of 3-[(2-amino-3-fluoro-4-pyridyl)methyl]-7-hydroxy-4-methyl- chromen-2-one (synthesis described in WO 2013/035754) (3 g, 9.99 mmol) in DMAc (30 mL) were added TEA (3.03 g, 29.97 mmol), CsF (2.28 g, 14.99 mmol) and 2,3- difluoropyridine (2.30 g, 19.98 mmol). The mixture was stirred at 80 °C for 16 h. The reaction mixture was quenched with H2O (10 mL) and extracted with EtOAc (100 mL x 3). 62 ME1\53438692.v1 136867-00920 The combined organic layers were washed with water (30 mL x 3), dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure. The residue was purified by flash chromatography on silica gel (MeOH in DCM = 0% - 5%) to give the 3-[(2-amino-3-fluoro- 4-pyridyl)methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one (1.6 g, 4.1 mmol, 40.5% yield) as a white solid.1H NMR (400 MHz, DMSO-d6) δ = 8.00-7.97 (m, 1H), 7.95- 7.86 (m, 2H), 7.58 (d, J = 5.2 Hz, 1H), 7.32-7.24 (m, 2H), 7.24-7.19 (m, 1H), 6.30-6.25 (m, 1H), 6.11 (s, 2H), 3.93 (s, 2H), 2.45 (s, 3H). To a solution of 3-[(2-amino-3-fluoro-4-pyridyl)methyl]-7-[(3-fluoro-2-pyridyl)oxy]- 4-methyl-chromen-2-one (100 mg, 252.9 umol) in THF (2 mL) was added NaH (50.6 mg, 1.3 mmol, 60% purity in oil) at 0°C. The mixture was stirred at 0 °C for 1 h. Then N- methylsulfamoyl chloride (36.1 mg, 278.2 umol) was added to the above mixture. The mixture was stirred at 25 °C for 16 h. The mixture was quenched with water (20 mL). The mixture was extracted with EtOAc (20 mL x 2). The organic layer was dried over anhydrous Na2SO4, filtered and concentrated. The crude was purified by flash column chromatography on silica gel (EtOAc in Dichloromethane = 0-40%) and prep-HPLC (column: Welch Xtimate C18150 x 25mm x 5um; mobile phase: [water(NH3H2O+NH4HCO3)-ACN]; B%: 35%-65%, 7 min) to give 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2- pyridyl)oxy]-4-methyl-chromen-2-one (6 mg, 12.3 umol, 4.9% yield) as white solid. 1H NMR (400 MHz, CD3CN) δ = 8.29 (br s, 1H), 7.98-7.95 (d, J = 4.8 Hz, 1H), 7.93-7.90 (m, 1H), 7.87-7.83 (m, 1H), 7.74-7.67 (m, 1 H), 7.25-7.17 (m, 3H), 6.88-6.83 (m, 1H), 5.85 (br s, 1H), 4.07 (s, 2H), 2.61 (s, 3H), 2.48 (s, 3H). 19F NMR (376.5 MHz, CDCl3) δ = -136.38, -141.72 ppm. LCMS Rt = 0.865 min, in 1.5 min chromatography, 5-95AB, ESI calcd. for C22H19N4F2O5S [M+H]+ 489.1, found 489.1. Preparation of Crystalline Form I of 3-[(2-amino-3-fluoro-4-pyridyl)methyl]-7- hydroxy-4-methyl-chromen-2-one N-methylsulfamoyl chloride (about 2.8 eq.) was added dropwise to a solution of dimethylformamide (about 10 vol.), acetonitrile (about 10 vol.), and pyridine (about 3 eq.) at a temperature of about 0°C to about 10°C. About 1 eq. of Compound 1 prepared according to the procedures described in PCT/US2023/019588 reproduced above, was added and the 63 ME1\53438692.v1 136867-00920 reaction was aged for about 2 hours. The reaction was then warmed to about 20 °C to about 30 °C and about 20 vol. of water was added, and the mixture was aged for about 0.5 hours. The solid was filtered and dried at about 40 °C to about 50°C to afford the crude product. The product was stirred in a mixture of dimethyl sulfoxide/acetonitrile (about 1 vol. / about 10 vol.) at about 20 °C to about 30 °C for about 2 hours. The mixture was filtered and the cake was dried for about 2 hours at about 40 °C to about 50 °C to afford crystalline Form I of 3- [[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4- methyl-chromen-2-one. Alternatively, Form I of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7- [(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one can also be obtained following the procedures described above and utilizing seeding to facilitate Form I isolation. An XRPD of Form I is shown in Figure 34A and TGA/DSC curves of the starting material are shown in Figure 34B. Material Instruments and Methods XRPD For XRPD analysis, Empyrean and X’pert3 X-ray powder diffractometers from Panalytical were used. Sample was spread on the middle of a zero-background Si holder. The XRPD parameters used are listed in Table . Table 1: Parameters for XRPD test Model Reflection mode VT-XRPD X-Ray wavelength Cu, kα, Kα1 (Å): 1.540598, Kα2 (Å): 1.544426 Kα2/Kα1 ratio: 0.50 X-Ray tube setting 45 kV, 40 mA 45 kV, 40 mA Divergence slit 1/8º 1/8º Scan mode Continuous Continuous Scan range (°2TH) 3~40 3~40 Scan step time (s) 46.67 33.02 Step size (°2TH) 0.0263 0.0167 Test time approximately 5 min 4 s Approximately 10 min 17 s TGA and DSC TGA data were collected using a Discovery TGA 5500/TGA 550 TGA from TA Instruments and DSC was performed using a Discovery DSC 2500/DSC 250 DSC from TA 64 ME1\53438692.v1 136867-00920 Instruments. Detailed parameters used are listed in Table . Table 2: Parameters for TGA and DSC test Parameters TGA DSC Method Ramp Ramp Sample pan Aluminum, open Aluminum, crimped Temperature RT~350 ºC 25 °C~300 ºC Heating rate 10 ºC/min 10 ºC/min Purge gas N2 N2 UPLC A Waters H-Class UPLC with PDA detector was utilized and detailed chromatographic conditions for purity and stoichiometric ratio analysis were listed in Table . Table 3: Chromatographic conditions UPLC Waters H-Class UPLC with PDA detector Column Acquity UPLC BEH C18, 50×2.1 mm, 1.7 µm A: 0.05% TFA in H2O Mobile phase B: 0.05% TFA in ACN Time (min) %B 0.0 20 10.0 40 Gradient table 13.0 90 13.1 20 15.0 20 Run time 15.0 min Post time 0.0 min Flow rate 0.5 mL/min Injection volume 2.4 μL Detector wavelength 278 nm Column temperature 30 ºC Sampler temperature RT Diluent ACN 65 ME1\53438692.v1 136867-00920 IC Thermo AQ RFIC and ThermoFisher ICS-1100 were utilized and detailed conditions were listed in Table and Table . Table 4: Ion chromatograph conditions and parameters for anion IC Thermo AQ RFIC Column Dionex IonPacTM AS11 HC Analytical (4 × 250 mm) Mobile phase 35 mM KOH Injection volume 25 μL Flow rate 1.0 mL/min Cell temperature 35 ºC Column temperature 35 ºC Current 87 mA Run time 12 min Table 5: Ion chromatograph conditions and parameters for cation IC ThermoFisher ICS-1100 Column Dionex IonPac™ CS12A RFIC™ 4×250mm Analytical Mobile phase 20 mM Methanesulfonic acid Injection volume 25 μL Flow rate 1.0 mL/min Cell temperature 35 ºC Column temperature 35 ºC Current 80 mA Run time 7~17 min 1H Solution NMR NMR was collected on Bruker 400MHz NMR Spectrometer in deuterated solvent. Salt Preparations 20 mg of starting material and corresponding counter-ions/co-formers were weighed into each HPLC vial with a molar charge ratio of 1:1, which was magnetically stirred 66 ME1\53438692.v1 136867-00920 (approximately 1000 rpm) at RT after the addition of the corresponding solvent for about three days. Solids were isolated for XRPD analysis. Multiple crystalline salt hits were obtained based on the XRPD comparison. Results are summarized in Table . All the salt hits were characterized by TGA, DSC, NMR and UPLC purity. The stoichiometry of salt hits was determined by NMR or ultra performance liquid chromatography combined with ion chromatography (hereinafter UPLC/IC). Characterization results of salt hits are listed in Table . Detailed preparation and characterization results are summarized below, under Polymorph Screening of Salt Leads. The structures of selected the counter-ions/co-formers used in the screening experiments are given in Figure 40. Table 6: Summary of salt screening results Solvent Co-former C: A: Acetone B: THF DMSO/EtOH D: ACN (1:3, v/v) Blank Free Form I[1] Free Form I[1] Free Form I[1] Free Form I[1] HCl salt Form HCl salt Form HCl salt Form HCl [1 Free Form I II ] III[1] I[1] 1,5- 1,5- 1,5- 1,5-Naphthalene- Naphthalenedi- Naphthalenedi- Free Form I[2] Naphthalenedi- disulfonic acid sulfonate Form sulfonate Form sulfonate Form I[1] I[2] II[1] 1,2- Edisylate Form Edisylate Form [2] Edisylate Form Ethanedisulfonic I[1] I[2] Free Form I II[1] acid HBr HBr salt Form Weak Fre [2] HBr salt Form I[1] crystallinity[5] e Form I II[1] KOH K salt Form II[1] K salt Form I[1] [1] K salt Form II NaOH Na salt Form Na salt Form Na salt Form Na salt F [1] I[1] orm I I II[1] III[6] Ca salt Form Ca salt For I + 2 [7] m Ca(OH) Ca salt Form I [7] Ca(OH) I 2 + II II [7] peaks[7] Choline salt Choline salt Choline salt Choline salt Form I[1] Form I[1] Form II[1] Form I[1] Diethylamine Diethylamine Diethylamine Diethylamine salt Form II[2] salt Form II[2] salt Form II[5] salt Form I[1] [1]: The samples were stirred at RT for 3 days. [2]: After slurrying at RT for 9 days, extra corresponding co-former was added into the samples (the molar charge of total co-formers/freeform was 5:1) and stirred at RT for 5~ 6 days. 67 ME1\53438692.v1 136867-00920 [5]: After slurrying at RT for 9 days, extra corresponding co-former was added into the samples (the molar charge of total co-formers/freeform was 5:1). After slurrying at RT for 2 days, clear solution was observed. The samples were slurried at 5 ºC for 4 days and a clear solution or limited solid was observed. Approximately 1 mL MTBE was added into the samples and stirred at RT overnight. [6]: After slurrying at RT for 7 days and at 5 ºC for 3 days, clear solution was observed. 1.2 mL MTBE was added into the sample and slurried at RT for 5 days. [7]: After slurrying at RT for 9 days, another equal molar amount of Free Form I was added into the samples and stirred at RT for approximately 6 days. Table 7: Characterization results of initial hits Molar ratio Residual (counter- UPLC TGA weight loss DSC endotherm Salt hit solvent ion or co- Purity (%) (ºC, peak) (wt%) former (Area%) /API)# 1.0 K salt Form I 1.86 (220 ºC) 249.7 1.0 97.69 (THF) K salt Form II 0.78 (160 ºC) 185.0, 246.4 0.6 0.8 98.44 3.24 (160-220 ºC) (ACN) K salt Form III 11.88 (180 ºC) 145.8, 165.4, 14.1 1.0 98.72 262.1 (DMSO) Na salt Form II 5.96 (180 ºC) 65.3, 118.5, 179.3 Not 1.1 98.28 detected 0.97 (140 ºC) Na salt Form III 17.04 (140-280 179.8 1.1 98.95 (DMSO) ºC) 0.2 Ca salt Form I 7.11 (180 ºC) 73.1, 135.8, 200.2 0.4 96.88 (Acetone) 73.0, 121.7, 4.0 Ca salt Form II 4.58 (190 ºC) 0.4 96.70 191.9, 236.4 (THF) 0.86 (150 ºC) 7.51 (150-210 ºC) 17.8 Ca salt Form III 11.36 (210-260 216.0 (DMSO) 0.5 98.81 ºC) Choline salt Form 1.37 (170 ºC) 63.8, 172.1 0.3 1.0 99.55 I & 91.6*, 160.2*, Not HCl salt Form IV 6.65 (150 ºC) 178.5 detected 0.3 97.13 1,5-Naphthalene- 0.6 disulfonate Form I 3.13 (150 ºC) 110.2, 185.0 (Acetone) 0.7 93.39 68 ME1\53438692.v1 136867-00920 Molar ratio Residual (counter- UPLC TGA weight loss DSC endotherm Salt hit solvent ion or co- Purity (%) (ºC, peak) (wt%) former (Area%) /API)# 1,5-Naphthalene- 130.9, 143.7*, 0.7 disulfonate Form 5.48 (150 ºC) II Not Edisylate Form I 2.84 (160 ºC) 80.1, 156.8, 170.5 0.8 91.94 detected Not Edisylate Form II 3.71 (160 ºC) 74.2, 116.5, 131.1 0.8 92.77 detected 81 & .9, 0.2 HBr salt Form I 9.40 (160 ºC) 0.7 98.01 146.8, 169.7 (Acetone) Not HBr salt Form II 2.61 (110 ºC) 76.3, 147.5 1.0 99.26 detected *: Exotherm, peak temperature. #: Determined by 1H NMR or UPLC/IC. &: Some peaks were consistent with Free Form I, suggesting that it may be a mixture of salt and Free Form I. Re-preparation of Certain Salts Based on the results of the initial salt screening, K salt Form I, Na salt Form II, Ca salt Form I, choline salt Form I and HBr salt Form II showed relatively good solid state properties. Hence, they were selected as the salt leads for scale-up. Detailed procedures for re- preparation of the salt leads are listed in Table . The XRPD comparison results confirmed that K salt Form I, Na salt Form II, Ca salt Form II, Choline salt Form I and HBr salt Form II were generated. Additional characterization results are summarized in Table . The re-prepared salt samples were used for polymorph screening experiments. Table 8: Re-Preparation procedures of salt leads Salt Lead Procedures 1. Weigh 439.8 mg Free Form I and 51.8 mg KOH into a 20-mL glass vial. Add 10 mL THF. K Form I 2. Magnetically stir at RT for 2 days. 3. Isolate the suspension by centrifugation. Dry solid at RT under vacuum overnight. A total of 421 mg solids (Yield: 88.5%) were obtained. 69 ME1\53438692.v1 136867-00920 Salt Lead Procedures 1. Weigh 439.5 mg Free Form I and 37.3 mg NaOH into a 20-mL glass vial. Add 10 mL ACN. 2. Magnetically stir at RT for 2 days. Na Form II 3. Isolate the suspension by centrifugation. Dry solid at RT under vacuum overnight. A total of 420 mg solids (Yield: 91.3%) were obtained. 1. Weigh 438.6 mg Free Form I and 33.8 mg Ca(OH)2 into a 20-mL glass vial. Add 10 mL acetone. 2. Magnetically stir at RT for 3 days and at 50 ºC for 3 days. Ca Form II 3. Isolate the suspension by centrifugation. Dry solid at RT under vacuum overnight. A total of 420 mg solids (Yield: 92.0%) were obtained. 1. Weigh 221.0 mg choline (aqueous solution, 45 wt%) into a 20-mL glass vial. Add 10 mL acetone. Then weigh 439.5 mg Free Form I into the vial. Choline salt Form I 2. Magnetically stir at RT for 3 days. 3. Isolate the suspension by centrifugation. Dry solid at RT under vacuum overnight. A total of 422 mg solids (Yield: 76.9%) were obtained. 1. Weigh 438.9 mg Free Form I into a 20-mL glass vial. Add 5 mL acetone. Then add 135 μL HBr solution (40%). HBr salt Form II 2. Magnetically stir at RT for 3 days. 3. Isolate the suspension by centrifugation. Dry solid at ambient condition overnight. A total of 426 mg solids (Yield: 83.2%) were #: Determined by 1H NMR or UPLC/IC. XRPD patterns of the re-prepared salt samples were consistent with XRPD patterns of reference materials (see Figures 35A, 36A, 37A, 38A, and 39A). DSC and TGA thermograms of the re-prepared salt samples are shown in Figures 35B, 36B, 37B, 38B, and 39B. 70 ME1\53438692.v1 136867-00920 Polymorph Screening of Certain Salts The re-prepared salt samples described above were used for polymorph screening experiments. General Methods Slurry at RT/50 ºC For each experiment, about 18 mg of the indicated starting material was suspended in 0.5 mL corresponding solvent in an HPLC glass vial. After the suspension was magnetically stirred at RT or 50 ºC (approximately 1000 rpm) for about 7 days, the remaining solids were isolated for XRPD analysis. Anti-solvent Addition For each experiment, about 18 mg of the indicated starting material was weighed into a 20-mL glass vial, followed by the addition of 0.4-0.6 mL corresponding solvent (e.g. DMSO) to dissolve the compound. If it was not completely dissolved, filter it to a new vial using a filter (PTFE, pore size of 0.45 μm). The solution obtained was magnetically stirred at the speed of 1000 rpm, followed by addition of anti-solvent (e.g. MTBE) stepwise till precipitate appeared or the total amount of anti-solvent reached 5.0 mL. The solids were isolated for XRPD analysis. Potassium Salt Forms A total of three forms of potassium salt of Compound 1 were observed from salt/co- crystal and polymorph screening experiments, named as K salt Forms I, II and III. XRPD patterns are displayed in Error! Reference source not found. 1A, 2A, and 3A, respectively. The XRPD overlay pattern for potassium salt Forms I, II and III is shown in Figure 3F. Additional characterization results are summarized in Table . Table 10: Characterization summary of K salt forms Crystal Weight loss in DSC Molar Solvent UPLC endotherm residu Speculated form TGA (%) ratio e purity form 71 ME1\53438692.v1 136867-00920 Crystal Weight loss in DSC Molar Solvent UPLC endotherm residue p Speculated form TGA (%) ratio urity form K Salt Form I Initial preparation of K salt Form I is described in the Salt Preparations section above. Characterization results are given in Table 7. As also described above (see Table 8), K salt Form I was re-prepared. As shown in overlay Figure 35A, the XRPD pattern of the re- prepared salt sample was consistent with that of the initial sample. The re-prepared material was used in further K salt polymorph screening. XRPD pattern of the re-prepared sample is shown in Figure 1A. XRPD peaks are listed in Table 11A. The NMR result in Error! Reference source not found. shows that the molar ratio of residual solvent THF/API was 0.05 (0.7 wt%). UPLC/IC results confirmed that the molar ratio of K+/freeform was 0.9 and the purity was 97.55 area %. The UPLC results are displayed in Table and in Error! Reference source not found.. VT-XRPD was performed for form identification and the results were shown in Error! Reference source not found.. No form change was observed after heating K salt Form I to 200 ºC and cooling to 25 ºC with N2 protection, indicating that K salt Form I was an anhydrate. Peak shift at 200 ºC may be caused by the expansion of crystal lattice at high temperature. Table 11A: Peaks list of K salt Form I 2θ [°] Rel [%] 4.5 75.1 7.3 38.1 8.9 82.0 10.6 30.0 14.6 79.6 16.4 16.3 17.2 100.0 17.8 81.2 19.3 43.5 22.1 38.0 22.4 33.7 23.5 53.4 72 ME1\53438692.v1 136867-00920 2θ [°] Rel [%] 23.8 77.5 32.2 25.5 36.1 7.1 Table 11B: UPLC result of K salt Form I # Peak RRT Area% # Peak RRT Area% 1 0.48 0.50 5 0.951 0.30 2 0.52 1.35 6 1.00 97.55 3 0.64 0.14 7 1.344 0.08 4 0.75 0.08 -- -- -- K Salt Form II K salt Form II was obtained via slurry of Compound 1 free Form I and equal molar KOH in ACN at RT for 3 days, followed by drying at RT under vacuum overnight. The XRPD result is shown in Error! Reference source not found.. Peaks are listed in Table 12A. UPLC/IC results showed that the molar ratio of K+/freeform was 1.0 and the purity was 97.68 area%. The UPLC results are displayed in Table and Error! Reference source not found.. TGA/DSC results in Error! Reference source not found. showed a weight loss of 1.95% up to 240 ºC and one endotherm at 257.9 ºC (peak temperature). 1H NMR result in Error! Reference source not found. revealed that the molar ratio of residual solvent ACN/API was 0.05 (0.6 wt%), suggesting that K salt Form II may be a hydrate or anhydrate. VT-XRPD was performed for form identification and the results are shown in Error! Reference source not found.. No form change was observed after heating K salt Form II to 200 ºC and cooling to 25 ºC with N2 protection (peak shift at 200 ºC may be caused by the expansion of crystal lattice at high temperature). KF result revealed that the content of water was 1.15%. Based on the results, K salt Form II was speculated to be an anhydrate. Table 11A: Peaks list of K salt Form II 73 ME1\53438692.v1 136867-00920 2θ [°] Rel [%] 4.4 43.7 7.8 24.4 8.6 42.0 10.8 10.9 12.9 18.4 13.7 19.1 14.4 81.5 17.2 37.7 17.5 100.0 18.4 41.8 18.9 26.2 21.5 44.8 22.8 3.6 23.5 35.4 24.0 54.1 27.6 31.5 28.0 7.7 30.1 16.5 30.4 10.6 31.1 22.3 32.2 9.1 33.9 10.8 36.6 16.5 Table 12B: UPLC result of K salt Form II # Peak RRT Area% # Peak RRT Area% 1 0.48 0.48 6 1.00 97.68 2 0.51 1.09 7 1.11 0.05 3 0.65 0.14 8 1.43 0.10 4 0.75 0.05 9 1.44 0.06 5 0.92 0.36 -- -- -- 74 ME1\53438692.v1 136867-00920 K Salt Form III K salt Form III was obtained via anti-solvent addition in DMSO/MTBE system at RT, followed by drying at RT under vacuum for approximately 23 hrs. XRPD and TGA/DSC results are shown in Error! Reference source not found. andError! Reference source not found., respectively. XRPD peaks are listed in Table 13A. TGA result showed a weight loss of 13.54% up to 130 ºC. DSC result showed three endotherms at 149.0, 161.3 and 267.5 ºC (peak temperature) NMR result in Error! Reference source not found. revealed that the molar ratio of residual solvent DMSO/API was 1.1 (approximately 14.4 wt%, close to the TGA weight loss). UPLC/IC results showed that the molar ratio of K+/freeform was 0.9 and the purity was 98.32 area%. UPLC results are displayed in Table and in Error! Reference source not found.. After heating K salt Form III to 170 ºC and cooling to RT, K salt Form II was obtained. VT-XRPD comparison results are displayed in Error! Reference source not found.. Based on the results, K salt Form III was proposed to be a DMSO mono-solvate. Table 12A: Peaks list of K salt Form III 2θ [°] Rel [%] 7.2 33.5 9.3 25.0 10.2 58.4 10.9 3.1 11.4 4.4 11.8 3.4 12.0 9.2 12.7 5.8 13.2 13.0 13.6 25.4 14.4 4.6 15.0 44.3 17.0 100.0 17.7 10.1 18.1 9.3 20.4 43.1 21.4 4.3 75 ME1\53438692.v1 136867-00920 2θ [°] Rel [%] 23.9 24.6 37.9 6.9 Table 13B: UPLC result of K salt Form III # Peak RRT Area% # Peak RRT Area% 1 0.48 0.53 4 0.92 0.19 2 0.51 0.89 5 1.00 98.32 3 0.65 0.07 -- -- -- Na Salt Forms A total of seven forms of sodium salt of Compound 1 were observed from salt/co- crystal and polymorph screening experiments, named as Na salt Forms I-VII. XRPD patterns of Forms I-VII are displayed in Figures 4H, 4A, 5A, 6, 7A, 8A, and 9A. Overlay XRPD results are shown in Figure 4G. Additional characterization results are summarized in Table 14. Table 14: Characterization summary of Na salt forms ystal form Weight lo DSC Molar Solvent UPLC Cr ss in Assigned TGA (%) endotherm ratio residue purity + form Na salt Form I Changed to Na salt Form II after drying. Not determined a salt Form IV Changed to amorphous after drying. Not determined Na Salt Form I After slurry of Compound 1 free Form I and equal molar NaOH in ACN at RT for 3 days, Na salt Form I was observed. XRPD results are shown in Error! Reference source not 76 ME1\53438692.v1 136867-00920 found.. After drying at RT under vacuum overnight, a slight form change was observed. Comparitive XRPD overlay is shown in Figure 4F. The form after drying was named as Na salt Form II. Na Salt Form II Initial preparation of Na Salt Form II is described in the Salt Preparations section above. Characterization results are given in Table 7. As also described above (see Table 8), Na Salt Form II was re-prepared. As shown in overlay Figure 36A, the XRPD pattern of the re-prepared salt sample was consistent with that of the initial sample. Additional characterization of the re-prepared sample is given in Tables 9 and 14. The re-prepared material was used in further Na salt polymorph screening. XRPD results of initially prepared batch of Na salt Form II are shown in Error! Reference source not found.. XRPD peaks are listed in Table 15A. UPLC/IC results showed that the molar ratio of Na+/freeform was 1.1 and the purity was 98.28 area%. UPLC results are displayed in Table 15B and in Figure 4D. TGA/DSC results of Na salt Form II are shown in Figure 4B. TGA result showed a weight loss of 5.96% up to 180 ºC. DSC result showed three endotherms at 65.3, 118.5 and 179.3 ºC (peak temperature) NMR result in Figure 4C showed negligible residual solvent ACN. VT-XRPD was performed for identification of Na salt Form II and the results are shown in Figure 4E. Form change was observed after N2 purging of Na salt Form II for 20 min at 25 ºC. After heating to 70 ºC with N2 protection, another new form was observed. After heating to 120 ºC and cooling to 25 ºC with N2 protection, a further slight form change was observed (highlighted by black stars). After exposure to ambient conditions, peaks of Na salt Form II (highlighted by red stars) was observed. Based on the results, Na salt Form II was proposed to be a hydrate. Table 15A: Peaks list of Na salt Form II 2θ [°] Rel [%] 6.5 100.0 7.6 22.5 8.4 12.6 11.5 6.9 14.7 21.0 15.2 28.7 17.1 18.3 77 ME1\53438692.v1 136867-00920 2θ [°] Rel [%] 18.0 18.7 18.9 4.8 19.5 6.6 20.9 6.0 22.9 87.6 Table 15B: UPLC result of Na salt Form # Peak RRT Area% # Peak 1 0.48 0.49 5 1.00 98.28 2 0.52 0.64 6 1.44 0.10 3 0.65 0.10 7 1.52 0.05 4 0.91 0.32 -- -- -- Na Salt Form III After slurrying of Compound 1 and equal molar NaOH in acetone at RT for 7 days and at 5 ºC for 3 days, followed by the addition of anti-solvent MTBE, slurrying at RT for 5 days and drying at RT under vacuum for approximately 6 hrs, Na salt Form III was obtained. XRPD result is shown in Figure 5A. XRPD peaks are listed in Table 16A. UPLC/IC results show that the molar ratio of Na+/freeform was 1.1 and the purity was 98.95 area%. UPLC results are displayed in Table 16B and in Figure 5D. TGA/DSC results are shown in Figure 5B. TGA result shows a weight loss of 0.97% up to 140 ºC and 17.04% between 140 ºC and 280 ºC. DSC result shows an endotherm at 179.8 ºC (peak temperature) NMR result in Figure 5C reveals that the molar ratio of residual solvent DMSO/API was 1.4 (17.5 wt%, close to the second step weight loss). After heating Na salt Form III to 200 ºC and cooling to RT, the sample melted. Based on the characterization results, Na salt Form III was proposed to be a DMSO mono-solvate. Table 16A: Peaks list of Na salt Form III 2θ [°] Rel [%] 4.8 8.1 9.7 52.4 9.9 76.2 78 ME1\53438692.v1 136867-00920 2θ [°] Rel [%] 12.9 18.6 13.2 49.8 13.5 8.2 14.1 8.7 14.5 1.5 15.3 100.0 15.6 35.0 16.4 33.6 16.6 46.4 16.9 21.7 17.2 28.1 17.8 89.5 18.2 21.8 18.6 53.3 19.0 64.1 20.3 26.5 21.0 42.7 21.6 14.1 22.0 31.9 22.5 37.0 22.9 72.9 23.6 60.6 24.3 29.7 28.7 11.7 29.0 28.1 29.9 13.0 30.8 11.2 33.1 12.9 36.3 11.5 37.6 8.3 79 ME1\53438692.v1 136867-00920 Table 16B: UPLC result of Na salt Form III # Peak RRT Area% 1 0.48 0.37 2 0.52 0.60 3 0.91 0.08 4 1.00 98.95 Na Salt Form IV Na salt Form IV was obtained by adding anti-solvent MTBE into a MeOH solution of Na salt Form II. After drying at RT under vacuum for approximately 23 hrs, it changed to mostly amorphous material. XRPD results of Form IV are shown in Error! Reference source not found.. XRPD Peaks of Form IV are listed in Table 17. Table 17: Peaks list of Na salt Form IV 2θ [°] Rel [%] 8.0 70.6 9.9 9.9 12.3 30.7 13.3 13.2 14.5 31.1 14.9 100.0 15.2 45.7 16.0 115.0 17.7 13.8 18.1 9.9 22.1 13.2 23.0 16.9 24.7 48.2 29.4 12.5 80 ME1\53438692.v1 136867-00920 Na Salt Form V Na salt Form V was obtained via slurry of Na salt Form II in NMP/2-MeTHF (1:4, v/v) at RT, followed by drying at RT under vacuum for approximately 8.5 hrs. XRPD results are shown in Figure 7A. XRPD peaks are listed in Table 18A. UPLC/IC results showed that the molar ratio of Na+/freeform was 1.0 and the purity was 99.61 area%. UPLC results are displayed in Table 18B and in Figure 7D. TGA/DSC results are shown in Figure 7B. TGA showed a weight loss of 2.92% up to 120 ºC and 14.99% between 120 ºC and 250 ºC. DSC result showed two endotherms at 112.0 and 134.8 ºC (peak temperature) NMR result in Figure 7C revealed that the molar ratio of residual solvent NMP/API was 0.9 (14.8 wt%, close to the second step weight loss). VT-XRPD was performed on Na salt Form V and the results are shown in Figure 7E. A form change was observed after N2 purging for 20 min at 25 ºC. No further form change was observed after heating to 112 ºC and cooling to 25 ºC with N2 protection. After exposure to ambient conditions for 30 min, Na salt Form V was re- obtained. Based on the results, Na salt Form V was speculated to be a hydrate. In addition, after heating Na salt Form V to 200 ºC and cooling to RT to remove the solvent NMP, the sample melted, suggesting that Na salt Form V also may be a NMP solvate. Based on the characterization results, Na salt Form V was proposed to be a water-NMP co-solvate. NMP may be removed after the sample melted. Table 18A: Peaks list of Form V 2θ [°] Rel [%] 8.6 8.7 9.3 17.1 9.6 51.5 10.8 35.7 11.2 9.0 11.6 6.0 12.9 5.5 13.4 4.1 13.6 5.6 14.6 23.6 15.5 10.6 16.2 94.6 16.9 26.4 81 ME1\53438692.v1 136867-00920 2θ [°] Rel [%] 17.2 21.4 17.5 50.3 17.9 32.6 18.4 29.9 18.8 16.7 19.0 30.0 19.7 100.0 20.9 10.6 22.1 35.6 22.8 16.5 23.3 43.3 23.5 25.2 24.3 37.7 28.4 6.0 28.7 9.7 29.5 21.3 31.3 8.3 32.7 8.6 33.8 0.5 Table 18B: UPLC result of Na salt Form V # Peak RRT Area% # Peak RRT Area% 1 0.48 0.19 3 1.00 99.61 2 0.51 0.12 4 1.49 0.08 Na Salt Form VI Na salt Form VI was obtained via slurry of Na salt Form II in DMAc/H2O (1:4, v/v) at RT for 7 days and 5 ºC for 4 days, followed by drying at RT under vacuum for 1 day. XRPD results are shown in Figure 8A. XRPD peaks are listed in Table 19A. UPLC/IC results showed that the molar ratio of Na+/freeform was 1.0 and the purity was 99.36 area%. UPLC results are displayed in Table 19B and in Figure 8D. TGA/DSC results are shown in Figure 8B. TGA result showed a stepwise weight loss of 13.48% up to 170 ºC. DSC result showed 82 ME1\53438692.v1 136867-00920 four endotherms at 49.9, 100.2, 116.9 and 154.6 ºC (peak temperature).1H NMR results in Figure 8C revealed that the molar ratio of residual solvent DMAc/API was 0.8 (11.5 wt%, close to the TGA weight loss). After heating Na salt Form VI to 200 ºC and cooling to RT, the sample melted. Based on the characterization results, Na salt Form VI was proposed to be a DMAc solvate. DMAc may be removed after the sample melted. Table 19A: Peaks list of Na salt Form VI 2θ [°] Rel [%] 6.4 23.8 10.6 100.0 10.9 6.7 11.6 13.0 11.8 7.9 12.9 37.4 13.1 18.4 14.4 99.7 15.2 27.5 16.2 52.1 17.2 23.0 18.3 44.0 19.3 47.7 19.6 71.0 20.4 21.8 21.4 22.5 22.5 13.9 22.9 60.0 23.3 47.9 24.5 12.8 29.0 24.9 30.7 18.5 83 ME1\53438692.v1 136867-00920 2θ [°] Rel [%] 32.8 8.6 38.0 9.7 Table 19B: UPLC result of Na salt Form VI # Peak RRT Area% # Peak RRT Area% 1 0.48 0.14 3 1.00 99.36 2 0.51 0.50 -- -- -- Na salt Form VII Na salt Form VII was obtained via slurry of Na salt Form II in acetone at RT for 7 days, followed by air-drying at RT. XRPD result is shown in Error! Reference source not found.. XRPD peaks are listed in Table 20A. UPLC/IC results showed that the molar ratio of Na+/freeform was 1.0 and the purity was 98.67 area%. UPLC results are displayed in Table and in Error! Reference source not found.. TGA/DSC results are shown in Error! Reference source not found.. TGA result showed a weight loss of 0.89% up to 110 ºC and 6.47% between 110 ºC and 170 ºC. DSC result showed two endotherms at 154.7 and 184.2 ºC (peak temperature) NMR result in Error! Reference source not found. revealed that the molar ratio of residual solvent acetone/API was 0.6 (6.6 wt%, close to the second step weight loss). After heating Na salt Form VII to 170 ºC and cooling to RT, amorphous sample (with two peaks) was obtained. XRPD comparison results are shown in Error! Reference source not found.. Based on the characterization results, Na salt Form VII was proposed to be an acetone solvate. Table 20A: Peaks list of Na salt Form VII 2θ [°] Rel [%] 9.6 100.0 9.9 48.4 12.9 30.1 15.0 6.5 15.5 84.7 16.4 14.0 17.2 75.5 84 ME1\53438692.v1 136867-00920 2θ [°] Rel [%] 18.1 71.7 19.2 39.5 19.8 31.3 21.1 16.4 21.2 17.3 21.5 31.0 22.3 48.6 23.2 87.9 29.0 45.7 30.0 7.7 31.1 20.3 32.0 20.8 34.5 17.8 35.3 15.5 Table 20B: UPLC result of Na salt Form VII # Peak RRT Area% # Peak RRT Area% 1 0.48 0.47 4 0.92 0.12 2 0.51 0.64 5 1.00 98.67 3 0.68 0.06 6 1.42 0.05 Ca Salt Forms A total of five forms of calcium salt of Compound 1 were observed from polymorph screening experiments, named as Ca salt Forms I-V. XRPD patterns are displayed in Figures 10A, 11A, 12A, 13A, and 14. The XPRD overlay pattern of Ca salt Forms I-V is displayed in Figure 10F. Additional characterization results are summarized in Table 21. Table 21: Characterization summary of Ca salt forms Crystal form Weight loss in DSC Molar Solvent UPLC endother Speculated TGA (%) m ratio residue purity form Ca salt Form III 0.66 (150 ºC) 216.0 0.5 17.8 98.81 DMSO 85 ME1\53438692.v1 136867-00920 Crystal form Weight loss in DSC Molar Solvent UPLC TGA (%) endotherm Speculated ratio residue purity (ºC, peak) (Ca2+/API) (wt%) (area%) form 7.51 (150-210 ºC) (DMSO) solvate Ca salt Form V Data not collected. Hydrate . Ca Salt Form I Ca salt Form I was generated as follows: 1) slurry of Compound 1 free Form I and equal molar Ca(OH)2 in acetone at RT for 9 days, 2) additional Compound 1 free Form I was added (the charge ratio of total freeform/Ca(OH)2 was 2:1) and slurry at RT for 5 days, 3) air- dry the sample at RT for 4 hrs, XRPD pattern is shown in Error! Reference source not found.. XRPD peaks are listed in Table 22A. UPLC/IC results confirmed that the molar ratio of Ca2+/freeform was 0.4 and the purity was 96.88 area%. UPLC results are displayed in Table and in Error! Reference source not found.. TGA/DSC results are shown in Error! Reference source not found.. TGA result showed a weight loss of 7.11% up to 180 ºC. DSC result showed three endotherms at 73.1, 135.8 and 200.2 ºC (peak temperature) NMR result in Error! Reference source not found. showed that the molar ratio of residual solvent acetone/API was 0.02 (0.2 wt%). VT-XRPD was performed for form identification and the results are displayed in Error! Reference source not found.. Form change was observed after N2 purging Ca salt Form I with N2 for 20 min at 25 ºC. After heating to 80 ºC, 150 ºC and cooling to 25 ºC with N2 protection, further form change was observed. After exposure to ambient conditions for approximately 30 min, Ca salt Form I was re-obtained. Based on the results, Ca salt Form I was proposed to be a hydrate. Table 22A: Peaks list of Ca salt Form I 2θ [°] Rel [%] 4.3 27.0 6.4 58.5 7.0 110.2 7.7 23.6 8.2 33.6 9.3 27.0 10.7 17.0 86 ME1\53438692.v1 136867-00920 2θ [°] Rel [%] 12.5 47.3 12.8 25.9 14.0 100.0 15.0 12.6 15.8 24.2 17.3 91.0 18.0 84.5 18.8 21.0 20.1 23.6 21.1 20.8 22.3 16.2 23.3 65.7 Table 22B: UPLC result of Ca salt Form I # Peak RRT Area% # Peak RRT Area% 1 0.48 0.48 6 0.95 0.06 2 0.52 1.89 7 1.00 96.88 3 0.65 0.16 8 1.37 0.06 4 0.75 0.09 9 1.43 0.11 5 0.92 0.29 -- -- -- Ca Salt Form II Initial preparation of Ca Salt Form II is described in the Salt Preparations section above. Characterization results are given in Table 7. As also described above (see Table 8), Ca Salt Form II was re-prepared. As shown in overlay Figure 37A, the XRPD pattern of the re-prepared salt sample was consistent with that of the initial sample. The re-prepared material was used in further Ca salt polymorph screening. XRPD pattern of the re-prepared sample is shown in Error! Reference source not found. XRPD peaks are listed in Table 23A. TGA/DSC results were shown in Error! Reference source not found.B. TGA result showed a weight loss of 2.18% up to 200 ºC. DSC result showed a broad endotherm at 93.0 ºC and a sharp endotherm at 253.9 ºC (peak temperature). The NMR result in Figure 11C 87 ME1\53438692.v1 136867-00920 showed that the molar ratio of residual solvent acetone/API was 0.02 (0.3 wt%). UPLC/IC result confirmed that the molar ratio of Ca2+/freeform was 0.4 and the purity was 98.83 area%. The UPLC results are displayed in Table 23B and in Error! Reference source not found.. VT-XRPD was performed for form identification and the results are shown in Error! Reference source not found.. No form change was observed after heating Ca salt Form II to 200 ºC and cooling to 25 ºC with N2 protection, indicating that Ca salt Form II was an anhydrate. Peak shift at 200 ºC may be caused by the expansion of the crystal lattice at high temperature. Table 23A: Peaks list of Ca salt Form II 2θ [°] Rel [%] 4.3 100.0 7.0 6.2 8.3 67.1 8.6 25.2 10.0 6.7 10.8 19.4 12.2 5.7 13.0 21.2 14.0 69.9 14.9 17.1 15.9 22.0 17.3 23.5 18.0 5.6 18.4 10.9 20.2 8.3 23.2 19.0 Table 23B: UPLC result of Ca salt Form II # Peak RRT Area% 1 0.48 0.54 2 0.52 0.56 3 0.91 0.07 88 ME1\53438692.v1 136867-00920 4 1.00 98.83 Ca Salt Form III Ca salt Form III was obtained via the following procedure: 1) slurry Compound 1 free Form I and equal molar Ca(OH)2 in DMSO/EtOH (1:3, v/v) at RT for 9 days, 2) additional Compound 1 free Form I was added (the charge ratio of extra freeform/Ca(OH)2 was 2:1) and slurry at RT for 5 days, 3) dry the sample at RT under vacuum for 6 hrs. XRPD pattern is shown in Figure 12A. XRPD peaks are listed in Table 24A. UPLC/IC results confirmed that the molar ratio of Ca2+/freeform was 0.5 and the purity was 98.81 area%. The UPLC results are displayed in Table 24B and in Error! Reference source not found.. TGA/DSC results are shown in Figure 12B. TGA showed a three-step weight loss of 0.86% (to 150 ºC), 7.51% (150-210 ºC) and 11.36% (210-260 ºC). DSC showed an endotherm at 216.0 ºC (peak temperature) NMR result in Figure 12C showed that the molar ratio of residual solvent DMSO/API was 1.4 (17.8 wt%). After heating Ca salt Form III to 200 ºC and cooling to RT, the sample partially melted. XRPD result in Figure 12E revealed that the remaining solid was almost amorphous (with weak peaks attributed to Ca salt Form III). Based on the results, Ca salt Form III was proposed to be a DMSO solvate. Table 24A: Peaks list of Ca salt Form III 2θ [°] Rel [%] 9.2 15.4 11.0 18.4 12.6 29.7 13.3 20.0 14.0 89.8 15.4 45.2 15.9 7.1 16.4 16.2 17.3 37.1 18.1 10.6 18.7 100.0 19.3 33.5 20.0 34.1 20.5 27.6 89 ME1\53438692.v1 136867-00920 2θ [°] Rel [%] 21.2 19.4 22.0 18.1 22.8 55.0 24.0 20.9 30.3 7.8 31.1 9.4 31.4 17.6 32.7 10.6 33.5 16.7 34.2 6.4 34.7 9.2 36.8 11.2 Table 24B: UPLC result of Ca salt Form III # Peak RRT Area% 1 0.48 0.18 2 0.52 0.83 3 0.91 0.11 4 1.00 98.81 5 1.43 0.07 Ca Salt Form IV/V Ca salt Form IV was obtained via the following procedure: after slurry of Ca salt Form II in MeOH/DCM (1:1, v/v) at RT for 7 days, clear solution was obtained. Solid was obtained after the solution became a slurry at 5 ºC for 1 day and at -20 ºC for 3 days. Air-dry the wet solid at RT for approximately 8 hrs. XRPD pattern is shown in Figure 13A. XRPD peaks are listed in Table 25A. UPLC/IC results confirmed that the molar ratio of Ca2+/freeform was 0.4 and the purity was 97.63 area%. UPLC results are displayed in Table 25B and in Figure 13D. TGA/DSC results were shown in Figure 13B. TGA showed a weight loss of 10.01% up to 190 ºC. DSC showed four endotherms at 65.7, 123.1, 174.7 and 186.4 ºC (peak temperature) NMR result in Figure 13C showed that the molar ratio of residual solvent MeOH/API was 0.2 (1.4 wt%). After storage of Ca salt Form IV at ambient 90 ME1\53438692.v1 136867-00920 conditions for 3 days, a form change was observed. The XRPD comparison results are shown in Figure 13E. The new form was named as Ca salt Form V. XRPD pattern is shown in Figure 14. XRPD peaks are listed in Table 25C. VT-XRPD was performed for identification of Ca salt Form V and the results are displayed in Figure 13F. No obvious form change was observed after N2 purging for 20 min at 25 ºC. After heating to 70 ºC, 125 ºC and cooling to 25 ºC with N2 protection, a form change was observed. After exposure to ambient conditions for approximately 30 min, Ca salt Form V was re-obtained. Based on the results, Ca salt Form V is proposed to be a hydrate. Table 25A: Peaks list of Ca salt Form IV 2θ [°] Rel [%] 6.6 92.5 7.4 63.7 8.4 31.7 11.2 32.7 12.6 34.3 13.1 19.2 13.6 20.2 14.4 16.5 14.8 34.4 15.9 12.6 16.8 22.5 17.5 82.5 18.2 18.5 21.1 25.9 22.2 100.0 23.3 33.2 35.2 11.1 91 ME1\53438692.v1 136867-00920 Table 25B: UPLC result of Ca salt Form IV # Peak RRT Area% # Peak RRT Area% 1 0.48 0.51 5 0.89 0.05 2 0.51 1.37 6 1.00 97.63 3 0.53 0.08 7 1.14 0.12 4 0.63 0.06 8 1.18 0.18 Table 25C: Peaks list of Ca salt Form V 2θ [°] Rel [%] 6.4 40.6 7.0 34.8 7.7 14.3 8.3 7.9 9.3 10.5 12.5 21.7 13.9 32.0 15.4 16.7 17.5 100.0 20.0 4.4 21.1 10.9 22.2 12.1 23.3 41.5 24.6 12.7 25.6 46.0 26.4 33.7 26.9 54.9 28.8 13.1 29.3 11.8 31.1 7.6 35.1 6.9 Choline Salt Forms A total of six forms of choline salt of Compound 1 were observed from polymorph 92 ME1\53438692.v1 136867-00920 screening experiments, named as Choline salt Forms I-VI. XRPD patterns are displayed in Figures 15A, 16, 17A, 18A, 19A, and 20A. XPRD overlay patterns of Choline salt Forms I- VI are displayed in Figure 15F. Additional characterization results are summarized in Table 26. Table 26: Characterization summary of Choline salt forms Crystal form Weight loss in DSC Molar Solvent UPLC TGA (%) endotherm Speculated ratio residue purity (ºC, peak) (base/API) (wt%) (area%) form Choline salt Form I 0.78 (180 ºC) 172.1 1.0 0.1 99.47 Anhydrate (re-prep batch) Choline salt 13 Form III 2.43 (150 ºC) 1.8, 135.3*, 175.7 1.1 1.9 (MeOH) 99.81 Anhydrate Choline salt 116.4, 142.3, EtOH 6.2 Form IV 7.02 (130 ºC) 144.6*, 176.2 (EtOH) solvate Choline salt Form V 2.17 (170 ºC) 142.2, 144.8*, 176.3 1.1 Not detected 99.93 Anhydrate Choline salt Form VI 1.27 (170 ºC) 174.6 1.1 1.1 (DMSO) 99.46 Anhydrate Choline salt Changed to Choline salt For To-be- Form II m VI after drying. determined *: Exotherm, peak temperature. Choline Salt Form I Initial preparation of Choline salt Form I is described in the Salt Preparations section above. Characterization results are given in Table 7. As also described above (see Table 8), Choline salt Form I was re-prepared. As shown in overlay Figure 38A, the XRPD pattern of the re-prepared salt sample was consistent with that of the initial sample. The re-prepared material was used in further choline salt polymorph screening. XRPD pattern of the re- prepared sample is shown in Error! Reference source not found. XRPD peaks are listed in Table 27A. TGA/DSC results in Figure 15B showed a weight loss of 0.78% up to 180 ºC and an endotherm at 172.1 ºC (peak temperature). The NMR result in Error! Reference source not found. revealed that the molar ratio of choline/freeform was 1.0 and residual solvent acetone/API was 0.01 (0.1 wt%). The UPLC purity was determined to be 99.47 area% and the results were displayed in Table 27B and in Figure 15D. VT-XRPD was performed for form identification and the results were shown in Figure 15E. No form change was observed after heating Choline salt Form I to 130 ºC and cooling to 25 ºC with N2 protection, indicating that Choline salt Form I was an anhydrate. Peak shift at 130 ºC may be caused by the expansion of the crystal lattice at high temperature. 93 ME1\53438692.v1 136867-00920 Table 3: Peaks list of Choline salt Form I 2θ [°] Rel [%] 4.3 5.5 8.6 8.8 9.4 3.3 11.2 38.8 12.8 34.4 13.6 4.3 14.1 44.3 14.4 10.9 15.2 3.1 15.5 5.3 15.9 6.6 16.4 26.7 16.7 34.0 17.1 100.0 18.2 12.7 18.9 24.2 20.4 75.0 21.4 99.8 22.5 20.9 22.9 16.1 23.4 27.4 24.1 6.8 28.4 45.6 28.9 7.7 29.5 4.6 31.2 5.5 32.5 3.8 33.7 3.4 34.6 9.0 35.5 18.1 38.0 5.0 94 ME1\53438692.v1 136867-00920 Table 27B: UPLC result of Choline salt Form I # Peak RRT Area% 1 0.48 0.19 2 0.52 0.34 3 1.00 99.47 Choline Salt Form II Choline salt Form II was obtained via slurry of Choline salt Form I in MeOH/MIBK (1:1) at 50 ºC for 7 days. XRPD pattern is shown in Error! Reference source not found. XRPD peaks are listed in Table 28. After drying at RT under vacuum overnight, a form change to Choline salt Form VI was observed (an extra peak marked by the black star was observed, see XRPD overlay in Figure 16B). Table 28: Peaks list of Choline salt Form II 2θ [°] Rel [%] 6.6 50.5 9.9 32.3 10.9 26.0 11.7 13.0 13.3 100.0 17.5 4.2 18.0 3.9 20.0 20.0 21.1 9.4 21.4 24.1 21.8 10.2 23.4 20.4 24.0 5.9 24.3 14.2 27.5 11.0 30.2 8.6 33.5 4.7 Choline Salt Form III 95 ME1\53438692.v1 136867-00920 Choline salt Form III was obtained via anti-solvent addition in MeOH/EtOAc system at RT, followed by air-drying at RT for approximately 23 hrs. XRPD results are shown in Figure 17A, and in Table 29A. TGA/DSC results are shown in Figure 17B. TGA showed a weight loss of 2.43% up to 150 ºC. DSC showed two endotherms at 131.8 and 175.7 ºC and an exotherm at 135.3 ºC (peak temperature) NMR in Figure 17C revealed that the molar ratio of choline/freeform was 1.1 and the residual solvent MeOH/API was 0.4 (1.9 wt%). UPLC result showed that the purity was 99.81 area%. UPLC results are listed in Table 29B and in Figure 17D. After heating Choline salt Form III to 110 ºC and cooling to RT, a mixture of Choline salt Form III+VI was observed (peaks of Choline salt Form VI were observed. Choline salt Form VI was identified to be an anhydrate). After heating Choline salt Form III to 140 ºC and cooling to RT, Choline salt Form VI was obtained. VT-XRPD comparison results are shown in Figure 17E. Negligible residual solvent (MeOH, marked by red box) was detected in the mixture of Choline salt Form III+VI (after heating to 110 ºC), so Choline salt Form III was not a solvate. Based on the characterization and heating results, Choline salt Form III was proposed to be an anhydrate. Table 29A: Peaks list of Choline salt Form III 2θ [°] Rel [%] 7.4 72.7 11.1 16.3 12.6 1.3 14.8 100.0 16.5 3.8 17.5 0.7 18.3 1.5 18.6 5.6 19.1 0.6 20.3 2.3 21.2 1.9 22.3 20.3 22.9 0.9 31.7 0.8 33.4 2.3 96 ME1\53438692.v1 136867-00920 Table 29B: UPLC result of Choline salt Form III # Peak RRT Area% 1 0.48 0.19 2 1.00 99.81 Choline Salt Form IV Choline salt Form IV was obtained via slurry of Choline salt Form I in EtOH at 50 ºC for 7 days, followed by air-drying at RT for approximately 8.5 hrs. XRPD results are shown in Figure 18A and in Table 30A. TGA/DSC results were shown in Figure 18B. TGA result showed a stepwise weight loss of 7.02% up to 130 ºC. DSC result showed three endotherms at 116.4, 142.3 and 176.2 ºC and an exotherm at 144.6 ºC (peak temperature) result in Figure 18C revealed that the molar ratio of choline/freeform was 1.1 and residual solvent EtOH/API was 0.9 (6.2 wt%, close to the TGA weight loss). UPLC result showed that the purity was 99.94 area%. UPLC results are listed in Table 30B and in Figure 18D. After heating Choline salt Form IV to 120 ºC and cooling to RT, a new form was obtained, which was named as Choline salt Form V. After heating Choline salt Form IV to 140 ºC and cooling to RT, Choline salt Form VI was obtained. The VT-XRPD comparison results were shown in Figure 18E. Based on the characterization and heating results, Choline salt Form IV was proposed to be an EtOH mono-solvate. Table 30A: Peaks list of Choline salt Form IV 2θ [°] Rel [%] 6.7 8.2 10.0 8.8 10.5 79.2 11.3 21.7 11.6 5.8 13.3 30.0 13.9 7.4 15.4 9.1 16.2 5.9 17.4 100.0 17.8 25.3 18.3 87.0 97 ME1\53438692.v1 136867-00920 2θ [°] Rel [%] 18.9 10.6 20.5 8.6 20.7 30.9 21.1 20.1 22.3 10.1 23.0 7.1 23.4 13.1 23.8 30.0 24.3 11.4 33.1 4.6 Table 30B: UPLC result of Choline salt Form IV # Peak RRT Area% 1 0.51 0.06 2 1.00 99.94 Choline Salt Form V Choline salt Form V was obtained via heating Choline salt Form IV to 120 ºC, cooling to RT and exposure to ambient conditions. XRPD results are shown in Figure 19A and in Table 31A. TGA/DSC results are shown in Figure 19B. TGA result showed a gradual weight loss of 2.17% up to 170 ºC. DSC result showed two endotherms at 142.2 and 176.3 ºC and an exotherm at 144.8 ºC (peak temperature) NMR result in Figure 19C revealed that the molar ratio of choline/freeform was 1.1 and negligible residual solvent was detected. UPLC result showed that the purity was 99.93 area%. UPLC results are listed in Table 31B and in Figure 19D. Based on the characterization results, Choline salt Form V may be an anhydrate. Table 4: Peaks list of Choline salt Form V 2θ [°] Rel [%] 7.3 11.2 10.6 89.8 10.9 9.4 98 ME1\53438692.v1 136867-00920 2θ [°] Rel [%] 11.4 27.9 14.5 41.0 15.0 5.8 15.6 20.1 16.2 11.7 16.9 11.4 17.4 100.0 17.8 23.3 18.6 86.4 19.8 26.0 20.7 42.3 21.2 41.3 22.0 7.5 23.3 13.5 24.2 23.3 Table 31B: UPLC result of Choline salt Form V # Peak RRT Area% 1 0.51 0.07 2 1.00 99.93 Choline Salt Form VI Choline salt Form VI was obtained via drying Choline salt Form II under vacuum at RT overnight. XRPD results are shown in Figure 20A and Table 32A. TGA/DSC results are shown in Figure 20B. TGA showed a gradual weight loss of 1.27% up to 170 ºC. DSC showed an endotherm at 174.6 NMR result in Figure 20C revealed that the molar ratio of choline/freeform was 1.1 and residual solvent DMSO/API was 0.09 (1.1 wt%). UPLC result showed that the purity was 99.46 area%. UPLC results are displayed in Table 32B and in Figure 20D. Based on the characterization results, Choline salt Form VI is proposed to be an anhydrate. Table 32A: Peaks list of Choline salt Form VI 99 ME1\53438692.v1 136867-00920 2θ [°] Rel [%] 9.5 7.9 11.2 50.9 11.4 13.7 12.9 15.3 14.1 24.7 14.4 29.6 15.3 6.2 16.1 30.1 16.4 100.0 16.7 23.2 17.0 41.7 17.8 9.9 18.1 6.0 18.9 27.8 19.3 36.4 19.7 14.4 20.0 39.7 20.4 64.3 21.1 26.7 22.1 12.5 22.4 31.2 22.9 49.2 23.4 11.4 23.7 8.9 28.3 6.6 33.2 7.9 Table 32B: UPLC result of Choline salt Form VI 100 ME1\53438692.v1 136867-00920 # Peak RRT Area% 1 0.49 0.09 2 0.51 0.39 3 0.92 0.05 4 1.00 99.46 Hydrogen Bromide (HBr) Salt Forms A total of three forms of HBr salt of Compound 1 were observed from polymorph screening experiments, named as HBr salt Forms I, II and III. XRPD patterns are displayed in Figures 21A, 22A, and 23. The XPRD overlay pattern of HBr salt Forms I-III is displayed in Figure 21E. Additional characterization results are summarized in Table 33. Table 33: Characterization summary of HBr salt forms m Weight loss in DSC Molar Solvent UPLC Crystal for Speculated TGA (%) endotherm ratio residue purity form determined *: Peaks of Compound 1 Form I were also observed, suggesting that the sample may be a mixture HBr salt (a new form) and freeform. HBr Salt Form I HBr salt Form I was obtained via slurry of Compound 1 free Form I and equal molar HBr in acetone at RT for 4 days and air-drying at RT overnight. XRPD results are shown in Figure 21A and Table 34A. TGA/DSC results are shown in Figure 21B. TGA showed a weight loss of 9.40% up to 160 ºC. DSC showed four endotherms at 81.9, 116.7, 146.8 and 169.7 ºC (peak temperature). As shown in Figure 21C, 1H NMR result showed that the molar ratio of residual solvent acetone/API was 0.02 (0.2 wt%). UPLC/IC results showed that the purity was 98.01 area% and the stoichiometric ratio of Br-/freeform was only 0.7. UPLC results are displayed in Table 34B and in Figure 21D. Table 34A: Peaks list of HBr salt Form I 2θ [°] Rel [%] 4.8 37.8 8.7 29.7 101 ME1\53438692.v1 136867-00920 2θ [°] Rel [%] 9.6 17.5 12.4 11.4 13.2 25.5 14.5 24.9 14.9 25.8 15.2 41.8 15.8 26.3 16.9 12.1 17.5 16.8 17.7 100.0 19.4 15.5 21.1 15.2 22.8 10.7 24.1 32.7 30.0 46.0 Table 34B: UPLC result of HBr salt Form I # Peak RRT Area% 1 0.52 1.93 2 1.00 98.01 3 1.43 0.07 HBr Salt Form II Initial preparation of HBr salt Form II is described in the Salt Preparations section above. Characterization results are given in Table 7. As also described above (see Table 8), HBr salt Form II was re-prepared. As shown in overlay Figure 39A, the XRPD pattern of the re- prepared salt sample was consistent with that of the initial sample. The re-prepared material was used in further HBr salt polymorph screening. XRPD pattern of the re-prepared sample is shown in Error! Reference source not found. XRPD peaks are listed in Table 35A. TGA/DSC curves are shown in Error! Reference source not found.. TGA showed a weight loss of 2.73% up to 120 ºC and two endotherms at 111.2 and 147.8 ºC (peak temperature). The 1H NMR result in Error! Reference source not found. showed that negligible residual 102 ME1\53438692.v1 136867-00920 solvent ACN was detected. UPLC/IC results confirmed that the molar ratio of Br-/freeform was 1.0 and the purity was 98.82 area%. The UPLC results are displayed in and in Error! Reference source not found.. VT-XRPD results in Error! Reference source not found. showed that form change was observed after N2 purging of HBr salt Form II at 25 ºC for 20 min. After heating to 110 ºC and cooling to 25 ºC with N2 protection, no further form change was observed (except for the intensity increase of peaks highlighted by the black stars). After exposure to ambient conditions, HBr salt Form II (with two additional peaks (highlighted by red stars) consistent with the sample after cooling to 25 ºC was re- obtained, indicating that HBr salt Form II was a hydrate (the theoretical water content of monohydrate was 3.0 wt%). Table 35A: Peaks list of HBr salt Form II 2θ [°] Rel [%] 4.9 58.1 6.8 11.8 9.7 19.5 10.8 33.9 12.8 5.5 13.7 7.1 14.5 35.1 15.3 100.0 15.6 24.5 16.3 7.7 17.4 14.3 19.4 26.3 20.5 8.5 21.6 12.1 22.9 4.9 23.6 27.5 24.2 29.8 28.6 5.0 29.2 12.5 29.7 4.7 30.8 12.8 103 ME1\53438692.v1 136867-00920 2θ [°] Rel [%] 31.7 5.8 34.2 4.2 35.3 4.0 Table 35B: UPLC result of HBr salt Form II # Peak RRT Area% 1 0.52 1.06 2 0.65 0.05 3 0.92 0.08 4 1.00 98.82 HBr Salt Form III HBr salt Form III was obtained via adding anti-solvent n-heptane into THF solution of HBr salt Form II. XRPD results are shown in Figure 23A and Table 36. After drying at ambient conditions, sample changed to HBr salt Form II. XRPD overlay results are shown in Figure 23B. Table 36: Peaks list of HBr salt Form III 2θ [°] Rel [%] 5.2 100.0 6.6 52.4 8.0 55.6 9.5 27.4 13.1 70.3 15.0 54.0 15.6 56.9 16.1 41.0 17.6 66.3 19.2 43.3 20.8 52.9 21.1 44.6 22.4 63.1 104 ME1\53438692.v1 136867-00920 2θ [°] Rel [%] 23.1 19.6 24.1 36.7 28.9 64.7 31.1 19.0 32.3 23.1 1,5-Naphthalenedisulfonate Salt Forms A total of two forms of 1,5-Naphthalenedisulfonate salt of Compound 1, named as 1,5-Naphthalenedisulfonate Form I and 1,5-Naphthalenedisulfonate Form II, were obtained from salt screening experiments. Characterization of Forms I and II is given below. 1,5-Naphthalenedisulfonate Salt Form I 1,5-Naphthalenedisulfonate Form I was obtained via slurry of Compound 1 free Form I and equal molar 1,5-naphthalenedisulfonic acid in acetone at RT for 3 days and drying at RT under vacuum overnight. XRPD results are shown in Figure 24A and Table 37A. TGA/DSC curves were shown in Figure 24B. TGA showed a weight loss of 3.13% up to 150 ºC. DSC showed two endotherms at 110.2 ºC and 185.0 ºC (peak temperature). As shown in Figure 24C, NMR result showed that the molar ratio of residual solvent acetone/API was 0.07 (0.6 wt%) and the stoichiometric ratio of acid/freeform was 0.7. As shown in Figure 24D and Table 37B, UPLC results confirmed that the purity was 93.39 area%. Table 37A: Peaks list of 1,5-Naphthalenedisulfonate Form I 2θ [°] Rel [%] 7.5 22.9 8.3 36.5 10.6 18.3 11.1 58.0 11.8 18.5 12.2 32.8 12.4 16.2 13.1 23.3 13.7 13.7 14.0 42.6 105 ME1\53438692.v1 136867-00920 2θ [°] Rel [%] 14.5 22.2 15.0 24.1 15.7 72.5 16.0 33.6 16.4 23.3 16.7 26.4 16.9 25.4 Table 37B: UPLC result of 1,5-Naphthalenedisulfonate Form I # Peak RRT Area% 1 0.52 6.31 2 0.65 0.13 3 0.91 0.07 4 1.00 93.39 5 1.44 0.11 1,5-Naphthalenedisulfonate Salt Form II 1,5-Naphthalenedisulfonate Form II was obtained via slurry of Compound 1 free Form I and equal molar 1,5-naphthalenedisulfonic acid in ACN at RT for 3 days and drying at RT under vacuum overnight. XRPD results are shown in Figure 25A and Table 38A. TGA/DSC curves are shown in Figure 25B. TGA showed a weight loss of 5.48% up to 150 ºC. DSC showed three endotherms at 130.9 ºC, 155.2 ºC and 164.3 ºC and one exotherm at 143.7 ºC (peak temperature). As shown in Figure 25C, NMR result showed that residual solvent ACN/API was 0.08 (0.7 wt%) and the stoichiometric ratio of acid/freeform was 0.9. As shown in Figure 25D and Table 38B, UPLC results confirmed that the purity was 90.82 area%. Table 38A: Peaks list of 1,5-Naphthalenedisulfonate Form II 2θ [°] Rel [%] 5.9 15.6 7.5 7.2 8.3 3.6 11.1 3.6 106 ME1\53438692.v1 136867-00920 2θ [°] Rel [%] 12.9 3.1 13.2 22.9 14.1 11.7 14.5 6.3 15.0 6.5 15.7 14.2 18.2 20.5 18.6 15.1 19.9 4.8 22.1 1.9 22.5 7.4 23.2 16.6 25.8 95.9 26.3 100.0 31.4 2.8 32.8 3.0 Table 38B: UPLC result of 1,5-Naphthalenedisulfonate Form II # Peak RRT Area% 1 0.51 8.83 2 0.64 0.10 3 0.91 0.14 4 1.00 90.82 5 1.44 0.10 1,2-Ethanedisulfonic (Edisylate) Salt Forms 107 ME1\53438692.v1 136867-00920 A total of two forms of Edisylate, named as Edisylate Form I and Edisylate Form II, were obtained from salt screening experiments. Characterization of Forms I and II is given below. Edisylate Salt Form I Edisylate Form I was obtained via slurry of Compound 1 free Form I and equal molar 1,2-ethanedisulfonic acid in acetone at RT for 3 days and drying at RT under vacuum overnight. XRPD results are shown in Figure 26A and Table 39A. TGA/DSC curves are shown in Figure 26B. TGA showed a weight loss of 2.84% up to 160 ºC. DSC showed three endotherms at 80.1, 156.8 and 170.5 ºC (peak temperature). As shown in Figure 26C, NMR result showed that negligible solvent acetone was detected and the stoichiometric ratio of acid/freeform was 0.8. As shown in Figure 26D and Table 39B, UPLC results confirmed that the purity was 91.94 area%. Table 59A: Peaks list of Edisylate Form I 2θ [°] Rel [%] 9.6 42.4 9.6 31.1 12.6 32.8 13.3 97.6 14.3 63.8 14.8 52.0 15.5 41.1 17.3 41.7 19.1 100.0 Table 39B: UPLC result of Edisylate Form I # Peak RRT Area% 1 0.52 7.83 2 0.65 0.12 3 1.00 91.94 4 1.39 0.05 5 1.44 0.07 Edisylate Salt Form II 108 ME1\53438692.v1 136867-00920 Edisylate Form II was obtained via slurry of Compound 1 free Form I and equal molar 1,2-ethanedisulfonic acid in ACN at RT for 3 days and drying at RT under vacuum overnight. XRPD results are shown in Figure 27A and Table 40A. TGA/DSC curves were shown in Figure 27B. TGA showed a weight loss of 3.71% up to 160 ºC. DSC showed three endotherms at three endotherms at 74.2, 116.5 and 131.1 ºC (peak temperature). As shown in Figure 27C, NMR result showed that negligible solvent ACN was detected and the stoichiometric ratio of acid/freeform was 0.8. As shown in Figure 27D and Table 40B, UPLC results confirmed that the purity was 92.77 area%. Table 40A: Peaks list of Edisylate Form II 2θ [°] Rel [%] 6.0 100.0 10.8 8.6 13.5 13.1 16.6 51.3 17.2 31.2 17.5 17.7 18.2 21.2 19.1 11.1 21.3 34.1 21.7 19.6 22.4 18.2 23.0 16.6 Table 40B: UPLC result of Edisylate Form II # Peak RRT Area% 1 0.52 6.97 2 0.64 0.07 3 0.91 0.05 4 1.00 92.77 5 1.09 0.07 6 1.44 0.07 Diethylamine Salt Forms 109 ME1\53438692.v1 136867-00920 A total of two forms of Diethylamine salt, named as Diethylamine salt Form I and Diethylamine salt Form II, were obtained from salt screening experiments. Characterization of Forms I and II is given below. Diethylamine Salt Form I Diethylamine salt Form I was obtained via slurry of Compound 1 free Form I and equal molar diethylamine in ACN at RT for 4 days. XRPD results are shown in Figure 28A and Table 41A. TGA/DSC curves are shown in Figure 28B. TGA showed a weight loss of 7.30% up to 100 ºC. DSC showed two endotherms at 98.7 ºC and 195.9 ºC (peak temperature). As shown in Figure 28C, NMR result showed that the molar ratio of residual solvent ACN/API was 0.4 (3.0 wt%) and the stoichiometric ratio of diethylamine/freeform was 0.5. As shown in Figure 28D and Table 41B, UPLC results confirmed that the purity was 99.22 area%. As shown in Figure 28E, after Diethylamine salt Form I was heated to 110 ºC, followed by being cooled down to RT and exposure to ambient conditions, Compound 1 free Form I was observed, suggesting that the TGA weight loss may be caused by the loss of diethylamine. Table 41A: Peaks list of Diethylamine salt Form I 2θ [°] Rel [%] 8.7 16.2 9.2 5.4 12.9 22.4 13.2 13.3 13.4 26.2 14.9 15.3 15.1 14.4 15.8 11.1 16.8 9.2 17.0 11.1 17.7 100.0 18.6 5.2 19.0 23.6 19.5 7.2 20.1 8.5 20.3 11.2 110 ME1\53438692.v1 136867-00920 2θ [°] Rel [%] 20.9 5.1 21.1 10.4 21.4 21.8 23.4 10.2 24.3 8.7 25.0 45.3 29.3 5.3 30.0 19.9 30.9 4.3 32.2 3.1 Table 41B: UPLC result of Diethylamine salt Form I # Peak RRT Area% 1 0.48 0.21 2 0.52 0.43 3 0.92 0.14 4 1.00 99.22 Diethylamine Salt Form II Diethylamine salt Form II was obtained via procedure as follows: 1) Slurry of Compound 1 free Form I and equal molar diethylamine in acetone at RT for 9 days; 2) Addition of another 4 times molar diethylamine and slurry at RT 5 days; 3) Air-dry the sample at RT for 4 hours. XRPD results are shown in Figure 29A and Table 42A. TGA/DSC curves are shown in Figure 29B. TGA showed a weight loss of 18.31% up to 160 ºC. DSC showed three endotherms at 119.8, 180.0 and 192.0 ºC (peak temperature). As shown in Figure 29C, NMR result showed that the molar ratio of residual solvent acetone/API was 0.2 (1.9 wt%) and the stoichiometric ratio of diethylamine/freeform was 0.9. As shown in Figure 29D and Table 42B, UPLC results confirmed that the purity was 99.62 area%. As shown in Figure 29E, after Diethylamine salt Form II was heated to 130 ºC, followed by being cooled down to RT and exposure to ambient conditions, Compound 1 free Form II was observed, suggesting that the TGA weight loss may be caused by the loss of diethylamine. Table 42A: Peaks list of Diethylamine salt Form II 111 ME1\53438692.v1 136867-00920 2θ [°] Rel [%] 3.7 15.4 7.3 18.1 8.5 4.5 10.3 6.7 11.0 100.0 12.3 15.7 13.8 18.6 14.6 42.8 16.9 23.7 17.9 36.2 18.2 12.2 20.9 4.3 22.9 7.0 23.5 3.6 Table 42B: UPLC result of Diethylamine salt Form II # Peak RRT Area% 1 0.48 0.09 2 0.52 0.24 3 0.92 0.05 4 1.00 99.62 Hydrogen Chloride (HCl) Salt Forms A total of four forms of HCl salt of Compound 1 was obtained. Initial salt screening provided HCl salt Forms I, II and III. During the re-preparation of HCl Form II/III, HCl salt Form IV was obtained. Characterization of Forms I-IV is given below. HCl Salt Form I HCl salt Form I was prepared via slurry of Compound 1 free Form I and equal molar HCl in ACN at RT for 4 days and air-drying at RT overnight. XRPD results are shown in Figure 30A and Table 43A. TGA/DSC curves are shown in Figure 30B. TGA showed a weight loss of 7.65% up to 150 ºC. DSC showed four endotherms at 93.9, 137.6, 153.4 and 112 ME1\53438692.v1 136867-00920 166.7 ºC (peak temperature). As shown in Figure 30C, 1H NMR result showed that the molar ratio of residual solvent ACN/API was 0.02 (0.2 wt%). UPLC and IC results confirmed that the purity was 98.34 area% and the stoichiometric ratio of Cl-/freeform was 0.6. UPLC results are shown in Figure 30D and Table 43B. Table 43A: Peaks list of HCl salt Form I 2θ [°] Rel [%] 4.8 89.3 6.8 24.2 9.7 19.5 10.7 9.3 12.3 4.1 13.5 5.8 14.4 20.2 15.3 100.0 15.9 19.5 17.3 6.3 19.4 24.4 21.7 10.2 24.1 34.4 29.2 19.6 30.9 12.2 Table 43B: UPLC result of HCl salt Form I # Peak RRT Area% 1 0.52 1.54 2 1.00 98.34 3 1.38 0.05 4 1.43 0.07 HCl Salt Form II HCl salt Form II was obtained via slurry of Compound 1 free Form I and equal molar HCl in acetone at RT for 3 days. XRPD results are shown in Figure 31 and Table 44. For further characterization, re-preparation was performed, but HCl salt Form IV was obtained. 113 ME1\53438692.v1 136867-00920 Characterization of Form IV is given below. Table 44: Peaks list of HCl salt Form II 2θ [°] Rel [%] 4.8 72.2 5.4 12.8 8.1 7.3 8.7 20.9 9.2 5.4 9.6 13.5 12.4 12.0 13.3 19.0 14.4 11.7 14.9 9.8 15.8 8.0 16.3 8.3 17.3 9.3 17.8 34.0 19.2 11.0 19.5 9.4 21.4 3.1 22.1 7.7 24.1 100.0 29.0 25.1 30.0 17.3 33.9 14.1 HCl Salt Form III HCl salt Form III was obtained via slurry of Compound 1 free Form I and equal molar HCl in THF at RT for 3 days. XRPD results are shown in Figure 32 and Table 45. After drying at RT under vacuum overnight, HCl salt Form I with a small amount of Compound 1 free Form I was observed. For further characterization, re-preparation was performed, but HCl salt Form IV was obtained. Characterization of Form IV is given below. Table 45: Peaks list of HCl salt Form III 114 ME1\53438692.v1 136867-00920 2θ [°] Rel [%] 4.8 97.6 6.3 63.9 8.1 43.1 8.7 61.0 9.6 26.5 10.8 6.7 13.3 17.5 14.2 77.4 15.8 22.9 16.5 92.1 17.4 26.4 17.8 15.1 19.2 47.4 19.5 16.2 20.3 38.7 21.7 13.9 22.7 11.9 23.1 14.8 23.5 100.0 24.1 58.3 25.1 31.0 28.6 7.9 30.0 49.4 30.4 10.5 32.3 11.3 33.9 6.4 HCl Salt Form IV HCl salt Form IV was obtained via slurry of Compound 1 free Form I and equal molar HCl in THF at RT for 4 days and air-drying at RT overnight. XRPD results are shown in Figure 33A and Table 46A. TGA/DSC curves were shown in Figure 33B. TGA showed a weight loss of 6.65% up to 150 ºC. DSC showed two exotherms at 91.6 ºC, 160.2 ºC and one endotherm at 178.5 ºC (peak temperature). As shown in Figure 33C, NMR result showed 115 ME1\53438692.v1 136867-00920 that no solvent residue was detected. UPLC and IC results confirmed that the purity was 97.13 area% and the stoichiometric ratio of Cl-/freeform was only 0.3. UPLC results were shown in Figure 33D and Table 46B. Overlay of the Compound 1 free Form I XRPD pattern with that of re-prepared Form IV before and after drying (Figure 33E) shows some peaks were consistent with Compound 1 free Form I, indicating that it may be a mixture of HCl salt and Compound 1 free Form I. Table 46A: Peaks list of HCl salt Form IV 2θ [°] Rel [%] 4.8 36.5 5.4 22.1 8.1 5.5 8.7 69.2 9.2 19.1 12.4 7.0 13.2 36.5 13.3 40.2 14.2 22.0 14.9 28.5 15.8 47.8 16.2 23.9 17.4 29.3 17.7 100.0 19.6 25.5 21.1 39.5 21.4 16.7 24.1 34.6 30.0 64.9 Table 46B: UPLC result of HCl salt Form IV 116 ME1\53438692.v1 136867-00920 # Peak RRT Area% 1 0.52 2.60 2 1.00 97.13 3 1.37 0.05 4 1.43 0.13 5 1.60 0.08 While a number of embodiments have been described, the scope of this disclosure is to be defined by the appended claims, and not by the specific embodiments that have been represented by way of example. The contents of all references (including literature references, issued patents, published patent applications, and co-pending patent applications) cited throughout this application are hereby expressly incorporated herein in their entireties by reference. Unless otherwise defined, all technical and scientific terms used herein are accorded the meaning commonly known to one with ordinary skill in the art. 117 ME1\53438692.v1

Claims

136867-00920 CLAIMS What is claimed is: 1. A potassium salt of the compound 3-[[3-fluoro-2-(methylsulfamoylamino)-4- pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one. 2. The potassium salt of Claim 1, wherein the potassium salt of the compound is crystalline. 3. The potassium salt of Claim 1 or 2, wherein the potassium salt of the compound is crystalline Form I characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 4.5°, 8.9°, 14.6°, 17.2°, 17.8°, 23.5°, and 23.8°. 4. The potassium salt of any one of Claims 1 to 3, wherein the potassium salt of the compound is crystalline Form I characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 4.5°, 8.9°, 14.6°, 17.2°, 17.8°, 23.5°, and 23.8°. 5. The potassium salt of any one of Claims 1 to 4, wherein the potassium salt of the compound is crystalline Form I characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 4.5°, 8.9°, 14.6°, 17.2°, 17.8°, 23.5°, and 23.8°. 6. The potassium salt of any one of Claims 1 to 5, wherein the potassium salt of the compound is crystalline Form I characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 4.5°, 8.9°, 14.6°, 17.2°, 17.8°, 23.5°, and 23.8°. 7. The potassium salt of any one of Claims 1 to 6, wherein the potassium salt of the compound is crystalline Form I characterized by x-ray powder diffraction peaks at 2θ angles 4.5°, 8.9°, 14.6°, 17.2°, 17.8°, 23.5°, and 23.8°. 8. The potassium salt of any one of Claims 1 to 7, wherein the potassium salt of the compound is crystalline Form I further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 7.3°, 10.6°, 19.3°, 22.1°, and 22.4°. 118 ME1\53438692.v1 136867-00920 9. The potassium salt of any one of Claims 1 to 8, wherein the potassium salt of the compound is characterized by an x-ray powder diffraction substantially similar to FIGURE 1A. 10. The potassium salt of any one of Claims 1 to 9, wherein the potassium salt of the compound is further characterized by a differential scanning calorimeter (DSC) thermogram comprising a peak endotherm at 246.1 °C ± 2 °C. 11. The potassium salt of any one of Claims 1 to 10, wherein the molar ratio of potassium counter-ion to compound is about 0.9. 12. The potassium salt of any one of Claims 1 to 11, wherein the potassium salt of the compound is an anhydrate. 13. The potassium salt of Claim 1 or 2, wherein the potassium salt is crystalline Form II characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 4.4°, 8.6°, 14.4°, 17.5°, 18.4°, 21.5°, and 24.0°. 14. The potassium salt of any one of Claims 1, 2, and 13, wherein the potassium salt is crystalline Form II characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 4.4°, 8.6°, 14.4°, 17.5°, 18.4°, 21.5°, and 24.0°. 15. The potassium salt of any one of Claims 1, 2, 13, and 14, wherein the potassium salt is crystalline Form II characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 4.4°, 8.6°, 14.4°, 17.5°, 18.4°, 21.5°, and 24.0°. 16. The potassium salt of any one of Claims 1, 2, and 13 to 15, wherein the potassium salt is crystalline Form II characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 4.4°, 8.6°, 14.4°, 17.5°, 18.4°, 21.5°, and 24.0°. 17. The potassium salt of any one of Claims 1, 2, and 13 to 16, wherein the potassium salt is crystalline Form II characterized by x-ray powder diffraction peaks at 2θ angles 4.4°, 8.6°, 14.4°, 17.5°, 18.4°, 21.5°, and 24.0°. 119 ME1\53438692.v1 136867-00920 18. The potassium salt of any one of Claims 1, 2, and 13 to 17, wherein the potassium salt of the compound is crystalline Form II further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 7.8°, 17.2°, 18.9°, 23.5°, and 27.6°. 19. The potassium salt of any one of Claims 1, 2, and 13 to 18, wherein the potassium salt is crystalline Form II characterized by an x-ray powder diffraction substantially similar to FIGURE 2A. 20. The potassium salt of any one of Claims 1, 2, and 13 to 19, wherein the potassium salt of the compound is further characterized by a differential scanning calorimeter (DSC) thermogram comprising a peak endotherm at 257.9 °C ± 2 °C. 21. The potassium salt of any one of Claims 1, 2, and 13 to 20, wherein the molar ratio of potassium counter-ion to compound is about 1. 22. The potassium salt of any one of Claims 1, 2, and 13 to 21, wherein the potassium salt of the compound is an anhydrate. 23. The potassium salt of Claim 1 or 2, wherein the potassium salt is crystalline Form III characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 7.2°, 9.3°, 10.2°, 13.6°, 15.0°, 17.0°, and 20.4°. 24. The potassium salt of any one of Claims 1, 2, and 23, wherein the potassium salt is crystalline Form III characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 7.2°, 9.3°, 10.2°, 13.6°, 15.0°, 17.0°, and 20.4°. 25. The potassium salt of any one of Claims 1, 2, 23, and 24, wherein the potassium salt is crystalline Form III characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 7.2°, 9.3°, 10.2°, 13.6°, 15.0°, 17.0°, and 20.4°. 120 ME1\53438692.v1 136867-00920 26. The potassium salt of any one of Claims 1, 2, and 23 to 25, wherein the potassium salt is crystalline Form III characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 7.2°, 9.3°, 10.2°, 13.6°, 15.0°, 17.0°, and 20.4°. 27. The potassium salt of any one of Claims 1, 2, and 23 to 26, wherein the potassium salt is crystalline Form III characterized by x-ray powder diffraction peaks at 2θ angles 7.2°, 9.3°, 10.2°, 13.6°, 15.0°, 17.0°, and 20.4°. 28. The potassium salt of any one of Claims 1, 2, and 23 to 27, wherein the potassium salt of the compound is crystalline Form III further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 12.0°, 13.2°, 17.7°, and 23.9°. 29. The potassium salt of any one of Claims 1, 2, and 23 to 28, wherein the potassium salt is crystalline Form III characterized by an x-ray powder diffraction substantially similar to FIGURE 3A. 30. The potassium salt of any one of Claims 1, 2, and 23 to 29, wherein the potassium salt of the compound is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 149.0 °C, 161.3 °C, and 267.5 °C ± 2 °C. 31. The potassium salt of any one of Claims 1, 2, and 23 to 30, wherein the molar ratio of potassium counter-ion to compound is about 0.9. 32. The potassium salt of any one of Claims 1, 2, and 23 to 31, wherein the potassium salt of the compound is a DMSO solvate. 33. A sodium salt of the compound 3-[[3-fluoro-2-(methylsulfamoylamino)-4- pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one. 34. The sodium salt of Claim 33, wherein the sodium salt of the compound is crystalline. 121 ME1\53438692.v1 136867-00920 35. The sodium salt of Claim 33 or 34, wherein the sodium salt of the compound is crystalline Form II characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 6.5°, 7.6°, 14.7°, 15.2°, and 22.9°. 36. The sodium salt of any one of Claims 33 to 35, wherein the sodium salt of the compound is crystalline Form II characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 6.5°, 7.6°, 14.7°, 15.2°, and 22.9°. 37. The sodium salt of any one of Claims 33 to 36, wherein the sodium salt of the compound is crystalline Form II characterized by x-ray powder diffraction peaks at 2θ angles 6.5°, 7.6°, 14.7°, 15.2°, and 22.9°. 38. The sodium salt of any one of Claims 33 to 37, wherein the sodium salt of the compound is crystalline Form II further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 8.4°, 17.1°, and 18.0°. 39. The sodium salt of any one of Claims 33 to 38, wherein the sodium salt of the compound is characterized by an x-ray powder diffraction substantially similar to FIGURE 4A. 40. The sodium salt of any one of Claims 33 to 39, wherein the sodium salt of the compound is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 65.3 °C, 118.5 °C, and 179.3 °C ± 2 °C. 41. The sodium salt of any one of Claims 33 to 40, wherein the molar ratio of sodium counter-ion to compound is about 1.1. 42. The sodium salt of any one of Claims 33 to 41, wherein the sodium salt of the compound is a hydrate. 43. The sodium salt of Claim 33 or 34, wherein the sodium salt is crystalline Form III characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 9.7°, 9.9°, 15.3°, 17.8°, 18.6°, 19.0°, 22.9°, and 23.6°. 122 ME1\53438692.v1 136867-00920 44. The sodium salt of any one of Claims 33, 34, and 43, wherein the sodium salt is crystalline Form III characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 9.7°, 9.9°, 15.3°, 17.8°, 18.6°, 19.0°, 22.9°, and 23.6°. 45. The sodium salt of any one of Claims 33, 34, 43, and 44, wherein the sodium salt is crystalline Form III characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 9.7°, 9.9°, 15.3°, 17.8°, 18.6°, 19.0°, 22.9°, and 23.6°. 46. The sodium salt of any one of Claims 33, 34, and 43 to 45, wherein the sodium salt is crystalline Form III characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 9.7°, 9.9°, 15.3°, 17.8°, 18.6°, 19.0°, 22.9°, and 23.6°. 47. The sodium salt of any one of Claims 33, 34, and 43 to 46, wherein the sodium salt is crystalline Form III characterized by at least seven x-ray powder diffraction peaks at 2θ angles selected from 9.7°, 9.9°, 15.3°, 17.8°, 18.6°, 19.0°, 22.9°, and 23.6°. 48. The sodium salt of any one of Claims 33, 34, and 43 to 47, wherein the sodium salt is crystalline Form III characterized by x-ray powder diffraction peaks at 2θ angles 9.7°, 9.9°, 15.3°, 17.8°, 18.6°, 19.0°, 22.9°, and 23.6°. 49. The sodium salt of any one of Claims 33, 34, and 43 to 48, wherein the sodium salt of the compound is crystalline Form III further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 13.2°, 15.6°, 16.4°, 16.6°, 21.0°, 22.0°, and 22.5°. 50. The sodium salt of any one of Claims 33, 34, and 43 to 49, wherein the sodium salt is crystalline Form III characterized by an x-ray powder diffraction substantially similar to FIGURE 5A. 51. The sodium salt of any one of Claims 33, 34, and 43 to 50, wherein the sodium salt of the compound is further characterized by a differential scanning calorimeter (DSC) thermogram comprising a peak endotherm at 179.8 °C ± 2 °C. 123 ME1\53438692.v1 136867-00920 52. The sodium salt of any one of Claims 33, 34, and 43 to 51, wherein the molar ratio of sodium counter-ion to compound is about 1.1. 53. The sodium salt of any one of Claims 33, 34, and 43 to 52, wherein the sodium salt of the compound is a DMSO solvate. 54. The sodium salt of Claim 33 or 34, wherein the sodium salt of the compound is crystalline Form IV characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 8.0°, 12.3°, 14.5°, 14.9°, 15.2°, 16.0°, and 24.7°. 55. The sodium salt of any one of Claims 33, 34, and 54, wherein the sodium salt of the compound is crystalline Form IV characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 8.0°, 12.3°, 14.5°, 14.9°, 15.2°, 16.0°, and 24.7°. 56. The sodium salt of any one of Claims 33, 34, 54, and 55, wherein the sodium salt is crystalline Form IV characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 8.0°, 12.3°, 14.5°, 14.9°, 15.2°, 16.0°, and 24.7°. 57. The sodium salt of any one of Claims 33, 34, and 54 to 56, wherein the sodium salt is crystalline Form IV characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 8.0°, 12.3°, 14.5°, 14.9°, 15.2°, 16.0°, and 24.7°. 58. The sodium salt of any one of Claims 33, 34, and 54 to 57, wherein the sodium salt of the compound is crystalline Form IV characterized by x-ray powder diffraction peaks at 2θ angles 8.0°, 12.3°, 14.5°, 14.9°, 15.2°, 16.0°, and 24.7°. 59. The sodium salt of any one of Claims 33, 34, and 54 to 58, wherein the sodium salt of the compound is crystalline Form IV further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 13.3°, 17.7°, 22.1°, 23.0°, and 29.4°. 124 ME1\53438692.v1 136867-00920 60. The sodium salt of any one of Claims 33, 34, and 54 to 59, wherein the sodium salt of the compound is characterized by an x-ray powder diffraction substantially similar to FIGURE 6. 61. The sodium salt of Claim 33 or 34, wherein the sodium salt is crystalline Form V characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 9.6°, 10.8°, 16.2°, 17.5°, 19.7°, 22.1°, 23.3°, and 24.3°. 62. The sodium salt of any one of Claims 33, 34, and 61, wherein the sodium salt is crystalline Form V characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 9.6°, 10.8°, 16.2°, 17.5°, 19.7°, 22.1°, 23.3°, and 24.3°. 63. The sodium salt of any one of Claims 33, 34, 61, and 62, wherein the sodium salt is crystalline Form V characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 9.6°, 10.8°, 16.2°, 17.5°, 19.7°, 22.1°, 23.3°, and 24.3°. 64. The sodium salt of any one of Claims 33, 34, and 61 to 63, wherein the sodium salt is crystalline Form V characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 9.6°, 10.8°, 16.2°, 17.5°, 19.7°, 22.1°, 23.3°, and 24.3°. 65. The sodium salt of any one of Claims 33, 34, and 61 to 64, wherein the sodium salt is crystalline Form V characterized by at least seven x-ray powder diffraction peaks at 2θ angles selected from 9.6°, 10.8°, 16.2°, 17.5°, 19.7°, 22.1°, 23.3°, and 24.3°. 66. The sodium salt of any one of Claims 33, 34, and 61 to 65, wherein the sodium salt is crystalline Form V characterized by x-ray powder diffraction peaks at 2θ angles 9.6°, 10.8°, 16.2°, 17.5°, 19.7°, 22.1°, 23.3°, and 24.3°. 67. The sodium salt of any one of Claims 33, 34, and 61 to 66, wherein the sodium salt of the compound is crystalline Form V further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 14.6°, 16.9°, 17.2°, 17.9°, 18.4°, 19.0°, 23.5°, and 29.5°. 125 ME1\53438692.v1 136867-00920 68. The sodium salt of any one of Claims 33, 34, and 61 to 67, wherein the sodium salt is crystalline Form V characterized by an x-ray powder diffraction substantially similar to FIGURE 7A. 69. The sodium salt of any one of Claims 33, 34, and 61 to 68, wherein the sodium salt of the compound is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 112.0 °C and 134.8 °C ± 2 °C. 70. The sodium salt of any one of Claims 33, 34, and 61 to 69, wherein the molar ratio of sodium counter-ion to compound is about 1.0. 71. The sodium salt of any one of Claims 33, 34, and 61 to 70, wherein the sodium salt of the compound is an H2O-NMP co-solvate. 72. The sodium salt of Claim 33 or 34, wherein the sodium salt is crystalline Form VI characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 8.5°, 10.6°, 14.4°, 16.2°, 19.3°, 19.6°, 22.9°, and 23.3°. 73. The sodium salt of any one of Claims 33, 34, and 72, wherein the sodium salt is crystalline Form VI characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 8.5°, 10.6°, 14.4°, 16.2°, 19.3°, 19.6°, 22.9°, and 23.3°. 74. The sodium salt of any one of Claims 33, 34, 72, and 73, wherein the sodium salt is crystalline Form VI characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 8.5°, 10.6°, 14.4°, 16.2°, 19.3°, 19.6°, 22.9°, and 23.3°. 75. The sodium salt of any one of Claims 33, 34, and 72 to 74, wherein the sodium salt is crystalline Form VI characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 8.5°, 10.6°, 14.4°, 16.2°, 19.3°, 19.6°, 22.9°, and 23.3°. 76. The sodium salt of any one of Claims 33, 34, and 72 to 75, wherein the sodium salt is crystalline Form VI characterized by at least seven x-ray powder diffraction peaks at 2θ angles selected from 8.5°, 10.6°, 14.4°, 16.2°, 19.3°, 19.6°, 22.9°, and 23.3°. 126 ME1\53438692.v1 136867-00920 77. The sodium salt of any one of Claims 33, 34, and 72 to 76, wherein the sodium salt is crystalline Form VI characterized by x-ray powder diffraction peaks at 2θ angles 8.5°, 10.6°, 14.4°, 16.2°, 19.3°, 19.6°, 22.9°, and 23.3°. 78. The sodium salt of any one of Claims 33, 34, and 72 to 77, wherein the sodium salt of the compound is crystalline Form VI further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 6.4°, 6.7°, 9.7°, 12.9°, 15.2°, 17.2°, 18.3°, 20.4°, 21.4°, and 29.0°. 79. The sodium salt of any one of Claims 33, 34, and 72 to 78, wherein the sodium salt is crystalline Form VI characterized by an x-ray powder diffraction substantially similar to FIGURE 8A. 80. The sodium salt of any one of Claims 33, 34, and 72 to 79, wherein the sodium salt of the compound is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 49.9 °C, 100.2 °C, 116.9 °C, and 154.6 °C ± 2 °C. 81. The sodium salt of any one of Claims 33, 34, and 72 to 80, wherein the molar ratio of sodium counter-ion to compound is about 1.0. 82. The sodium salt of any one of Claims 33, 34, and 72 to 81, wherein the sodium salt of the compound is a DMAc solvate. 83. The sodium salt of Claim 33 or 34, wherein the sodium salt is crystalline Form VII characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 9.6°, 9.9°, 15.5°, 17.2°, 18.1°, 22.3°, 23.2°, and 29.0°. 84. The sodium salt of any one of Claims 33, 34, and 83, wherein the sodium salt is crystalline Form VII characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 9.6°, 9.9°, 15.5°, 17.2°, 18.1°, 22.3°, 23.2°, and 29.0°. 127 ME1\53438692.v1 136867-00920 85. The sodium salt of any one of Claims 33, 34, 83, and 84, wherein the sodium salt is crystalline Form VII characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 9.6°, 9.9°, 15.5°, 17.2°, 18.1°, 22.3°, 23.2°, and 29.0°. 86. The sodium salt of any one of Claims 33, 34, and 83 to 85, wherein the sodium salt is crystalline Form VII characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 9.6°, 9.9°, 15.5°, 17.2°, 18.1°, 22.3°, 23.2°, and 29.0°. 87. The sodium salt of any one of Claims 33, 34, and 83 to 86, wherein the sodium salt is crystalline Form VII characterized by at least seven x-ray powder diffraction peaks at 2θ angles selected from 9.6°, 9.9°, 15.5°, 17.2°, 18.1°, 22.3°, 23.2°, and 29.0°. 88. The sodium salt of any one of Claims 33, 34, and 83 to 87, wherein the sodium salt is crystalline Form VII characterized by x-ray powder diffraction peaks at 2θ angles 9.6°, 9.9°, 15.5°, 17.2°, 18.1°, 22.3°, 23.2°, and 29.0°. 89. The sodium salt of any one of Claims 33, 34, and 83 to 88, wherein the sodium salt of the compound is crystalline Form VII further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 12.9°, 19.2°, 19.8°, 21.5°, 31.1°, and 32.0°. 90. The sodium salt of any one of Claims 33, 34, and 83 to 89, wherein the sodium salt is crystalline Form VII characterized by an x-ray powder diffraction substantially similar to FIGURE 9A. 91. The sodium salt of any one of Claims 33, 34, and 83 to 90, wherein the sodium salt of the compound is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 154.7 °C, and 184.2 °C ± 2 °C. 92. The sodium salt of any one of Claims 33, 34, and 83 to 91, wherein the molar ratio of sodium counter-ion to compound is about 1.0. 93. The sodium salt of any one of Claims 33, 34, and 83 to 92, wherein the sodium salt of the compound is an acetone solvate. 128 ME1\53438692.v1 136867-00920 94. A calcium salt of the compound 3-[[3-fluoro-2-(methylsulfamoylamino)-4- pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one. 95. The calcium salt of Claim 94, wherein the calcium salt of the compound is crystalline. 96. The calcium salt of Claim 94 or 95, wherein the calcium salt of the compound is crystalline Form I characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 6.4°, 7.0°, 12.5°, 14.0°, 17.3°, 18.0°, and 23.3°. 97. The calcium salt of any one of Claims 94 to 96, wherein the calcium salt of the compound is crystalline Form I characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 6.4°, 7.0°, 12.5°, 14.0°, 17.3°, 18.0°, and 23.3°. 98. The calcium salt of any one of Claims 94 to 97, wherein the calcium salt of the compound is crystalline Form I characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 6.4°, 7.0°, 12.5°, 14.0°, 17.3°, 18.0°, and 23.3°. 99. The calcium salt of any one of Claims 94 to 98, wherein the calcium salt of the compound is crystalline Form I characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 6.4°, 7.0°, 12.5°, 14.0°, 17.3°, 18.0°, and 23.3°. 100. The calcium salt of any one of Claims 94 to 99, wherein the calcium salt of the compound is crystalline Form I characterized by x-ray powder diffraction peaks at 2θ angles 6.4°, 7.0°, 12.5°, 14.0°, 17.3°, 18.0°, and 23.3°. 101. The calcium salt of any one of Claims 94 to 100, wherein the calcium salt of the compound is crystalline Form I further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 4.3°, 7.7°, 8.2°, 9.3°, 12.8°, 15.8°, 18.8°, 20.1°, and 21.1°. 102. The calcium salt of any one of Claims 94 to 101, wherein the calcium salt of the compound is characterized by an x-ray powder diffraction substantially similar to FIGURE 10A. 129 ME1\53438692.v1 136867-00920 103. The calcium salt of any one of Claims 94 to 102, wherein the calcium salt of the compound is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 73.1 °C, 135.8 °C and 200.2 °C ± 2 °C. 104. The calcium salt of any one of Claims 94 to 103, wherein the molar ratio of calcium counter-ion to compound is about 0.4. 105. The calcium salt of any one of Claims 94 to 104, wherein the calcium salt of the compound is a hydrate. 106. The calcium salt of Claim 94 or 95, wherein the calcium salt of the compound is crystalline Form II characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 4.3°, 8.3°, 8.6°, 13.0°, 14.0°, 15.9°, and 17.3°. 107. The calcium salt of any one of Claims 94, 95, and 106 wherein the calcium salt of the compound is crystalline Form II characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 4.3°, 8.3°, 8.6°, 13.0°, 14.0°, 15.9°, and 17.3°. 108. The calcium salt of any one of Claims 94, 95, 106, and 107, wherein the calcium salt of the compound is crystalline Form II characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 4.3°, 8.3°, 8.6°, 13.0°, 14.0°, 15.9°, and 17.3°. 109. The calcium salt of any one of Claims 94, 95, and 106 to 108, wherein the calcium salt of the compound is crystalline Form II characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 4.3°, 8.3°, 8.6°, 13.0°, 14.0°, 15.9°, and 17.3°. 110. The calcium salt of any one of Claims 94, 95, and 106 to 109, wherein the calcium salt of the compound is crystalline Form II characterized by x-ray powder diffraction peaks at 2θ angles 4.3°, 8.3°, 8.6°, 13.0°, 14.0°, 15.9°, and 17.3°. 130 ME1\53438692.v1 136867-00920 111. The calcium salt of any one of Claims 94, 95, and 106 to 110, wherein the calcium salt of the compound is crystalline Form II further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 10.8°, 14.9°, 18.4°, and 23.2°. 112. The calcium salt of any one of Claims 94, 95, and 106 to 111, wherein the calcium salt of the compound is characterized by an x-ray powder diffraction substantially similar to FIGURE 11A. 113. The calcium salt of any one of Claims 94, 95 and 106 to 112, wherein the calcium salt of the compound is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 93.0 °C and 253.9 °C ± 2 °C. 114. The calcium salt of any one of Claims 94, 95, and 106 to 113, wherein the molar ratio of calcium counter-ion to compound is about 0.4. 115. The calcium salt of any one of Claims 94, 95, and 106 to 114, wherein the calcium salt of the compound is an anhydrate. 116. The calcium salt of Claim 94 or 95, wherein the calcium salt of the compound is crystalline Form III characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 14.0°, 15.4°, 17.3°, 18.7°, 19.3°, 20.0°, and 22.8°. 117. The calcium salt of any one of Claims 94, 95, and 116 wherein the calcium salt of the compound is crystalline Form III characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 14.0°, 15.4°, 17.3°, 18.7°, 19.3°, 20.0°, and 22.8°. 118. The calcium salt of any one of Claims 94, 95, 116, and 117, wherein the calcium salt of the compound is crystalline Form III characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 14.0°, 15.4°, 17.3°, 18.7°, 19.3°, 20.0°, and 22.8°. 119. The calcium salt of any one of Claims 94, 95 and 116 to 118, wherein the calcium salt of the compound is crystalline Form III characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 14.0°, 15.4°, 17.3°, 18.7°, 19.3°, 20.0°, and 22.8°. 131 ME1\53438692.v1 136867-00920 120. The calcium salt of any one of Claims 94, 95, and 116 to 119, wherein the calcium salt of the compound is crystalline Form III characterized by x-ray powder diffraction peaks at 2θ angles 14.0°, 15.4°, 17.3°, 18.7°, 19.3°, 20.0°, and 22.8°. 121. The calcium salt of any one of Claims 94, 95, and 116 to 120, wherein the calcium salt of the compound is crystalline Form III further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 12.6°, 13.3°, 20.5°, and 24.0°. 122. The calcium salt of any one of Claims 94, 95, and 116 to 121, wherein the calcium salt of the compound is characterized by an x-ray powder diffraction substantially similar to FIGURE 12A. 123. The calcium salt of any one of Claims 94, 95, and 116 to 122, wherein the calcium salt of the compound is further characterized by a differential scanning calorimeter (DSC) thermogram comprising a peak endotherm at 216.0 °C ± 2 °C. 124. The calcium salt of any one of Claims 94, 95, and 116 to 123, wherein the molar ratio of calcium counter-ion to compound is about 0.5. 125. The calcium salt of any one of Claims 94, 95, and 116 to 124, wherein the calcium salt of the compound is a DMSO solvate. 126. The calcium salt of Claim 94 or 95, wherein the calcium salt of the compound is crystalline Form IV characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 6.6°, 7.4°, 8.4°, 11.2°, 12.6°, 14.8°, 17.5°, 22.2°, and 23.3°. 127. The calcium salt of any one of Claims 94, 95, and 126 wherein the calcium salt of the compound is crystalline Form IV characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 6.6°, 7.4°, 8.4°, 11.2°, 12.6°, 14.8°, 17.5°, 22.2°, and 23.3°. 132 ME1\53438692.v1 136867-00920 128. The calcium salt of any one of Claims 94, 95, 126, and 127, wherein the calcium salt of the compound is crystalline Form IV characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 6.6°, 7.4°, 8.4°, 11.2°, 12.6°, 14.8°, 17.5°, 22.2°, and 23.3°. 129. The calcium salt of any one of Claims 94, 95, and 126 to 128, wherein the calcium salt of the compound is crystalline Form IV characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 6.6°, 7.4°, 8.4°, 11.2°, 12.6°, 14.8°, 17.5°, 22.2°, and 23.3°. 130. The calcium salt of any one of Claims 94, 95, and 126 to 129, wherein the calcium salt of the compound is crystalline Form IV characterized by at least seven x-ray powder diffraction peaks at 2θ angles selected from 6.6°, 7.4°, 8.4°, 11.2°, 12.6°, 14.8°, 17.5°, 22.2°, and 23.3°. 131. The calcium salt of any one of Claims 94, 95, and 126 to 130, wherein the calcium salt of the compound is crystalline Form IV characterized by at least eight x-ray powder diffraction peaks at 2θ angles selected from 6.6°, 7.4°, 8.4°, 11.2°, 12.6°, 14.8°, 17.5°, 22.2°, and 23.3°. 132. The calcium salt of any one of Claims 94, 95, and 126 to 131, wherein the calcium salt of the compound is crystalline Form IV characterized by x-ray powder diffraction peaks at 2θ angles 6.6°, 7.4°, 8.4°, 11.2°, 12.6°, 14.8°, 17.5°, 22.2°, and 23.3°. 133. The calcium salt of any one of Claims 94, 95, and 126 to 132, wherein the calcium salt of the compound is crystalline Form IV further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 13.6°, 16.8°, 21.1°, and 35.2°. 134. The calcium salt of any one of Claims 94, 95, and 126 to 133, wherein the calcium salt of the compound is characterized by an x-ray powder diffraction substantially similar to FIGURE 13A. 135. The calcium salt of any one of Claims 94, 95, and 126 to 134, wherein the calcium salt of the compound is further characterized by a differential scanning calorimeter (DSC) 133 ME1\53438692.v1 136867-00920 thermogram comprising peak endotherms at 65.7 °C, 123.1 °C, 174.7 °C and 186.4 °C ± 2 °C. 136. The calcium salt of any one of Claims 94, 95, and 126 to 135, wherein the molar ratio of calcium counter-ion to compound is about 0.4. 137. The calcium salt of Claim 94 or 95, wherein the calcium salt of the compound is crystalline Form V characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 6.4°, 7.0°, 12.5°, 13.9°, 17.5°, 23.3°, 25.6°, 26.4°, and 26.9°. 138. The calcium salt of any one of Claims 94, 95, and 137 wherein the calcium salt of the compound is crystalline Form V characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 6.4°, 7.0°, 12.5°, 13.9°, 17.5°, 23.3°, 25.6°, 26.4°, and 26.9°. 139. The calcium salt of any one of Claims 94, 95, 137, and 138, wherein the calcium salt of the compound is crystalline Form V characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 6.4°, 7.0°, 12.5°, 13.9°, 17.5°, 23.3°, 25.6°, 26.4°, and 26.9°. 140. The calcium salt of any one of Claims 94, 95, and 137 to 139, wherein the calcium salt of the compound is crystalline Form V characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 6.4°, 7.0°, 12.5°, 13.9°, 17.5°, 23.3°, 25.6°, 26.4°, and 26.9°. 141. The calcium salt of any one of Claims 94, 95, and 137 to 140, wherein the calcium salt of the compound is crystalline Form V characterized by at least seven x-ray powder diffraction peaks at 2θ angles selected from 6.4°, 7.0°, 12.5°, 13.9°, 17.5°, 23.3°, 25.6°, 26.4°, and 26.9°. 142. The calcium salt of any one of Claims 94, 95, and 137 to 141, wherein the calcium salt of the compound is crystalline Form V characterized by at least eight x-ray powder diffraction peaks at 2θ angles selected from 6.4°, 7.0°, 12.5°, 13.9°, 17.5°, 23.3°, 25.6°, 26.4°, and 26.9°. 134 ME1\53438692.v1 136867-00920 143. The calcium salt of any one of Claims 94, 95, and 137 to 142, wherein the calcium salt of the compound is crystalline Form V characterized by x-ray powder diffraction peaks at 2θ angles 6.4°, 7.0°, 12.5°, 13.9°, 17.5°, 23.3°, 25.6°, 26.4°, and 26.9°. 144. The calcium salt of any one of Claims 94, 95, and 137 to 143, wherein the calcium salt of the compound is crystalline Form V further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 7.7°, 9.3°, 15.4°, 21.1°, 22.2°, 24.6°, 28.8°, and 29.3°. 145. The calcium salt of any one of Claims 94, 95, and 137 to 144, wherein the calcium salt of the compound is characterized by an x-ray powder diffraction substantially similar to FIGURE 14. 146. The calcium salt of any one of Claims 94, 95, and 137 to 145, wherein the calcium salt of the compound is a hydrate. 147. A choline salt of the compound 3-[[3-fluoro-2-(methylsulfamoylamino)-4- pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one. 148. The choline salt of Claim 147, wherein the choline salt of the compound is crystalline. 149. The choline salt of Claim 147 or 148, wherein the choline salt of the compound is crystalline Form I characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 11.2°, 12.8°, 14.1°, 16.7°, 17.1°, 20.4°, 21.4°, and 28.4°. 150. The choline salt of any one of Claims 147 to 149, wherein the choline salt of the compound is crystalline Form I characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 11.2°, 12.8°, 14.1°, 16.7°, 17.1°, 20.4°, 21.4°, and 28.4°. 151. The choline salt of any one of Claims 147 to 150, wherein the choline salt of the compound is crystalline Form I characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 11.2°, 12.8°, 14.1°, 16.7°, 17.1°, 20.4°, 21.4°, and 28.4°. 135 ME1\53438692.v1 136867-00920 152. The choline salt of any one of Claims 147 to 151, wherein the choline salt of the compound is crystalline Form I characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 11.2°, 12.8°, 14.1°, 16.7°, 17.1°, 20.4°, 21.4°, and 28.4°. 153. The choline salt of any one of Claims 147 to 152, wherein the choline salt of the compound is crystalline Form I characterized by at least seven x-ray powder diffraction peaks at 2θ angles selected from 11.2°, 12.8°, 14.1°, 16.7°, 17.1°, 20.4°, 21.4°, and 28.4°. 154. The choline salt of any one of Claims 147 to 153, wherein the choline salt of the compound is crystalline Form I characterized by x-ray powder diffraction peaks at 2θ angles 11.2°, 12.8°, 14.1°, 16.7°, 17.1°, 20.4°, 21.4°, and 28.4°. 155. The choline salt of any one of Claims 147 to 154, wherein the choline salt of the compound is crystalline Form I further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 16.4°, 18.9°, 22.5°, and 23.4°. 156. The choline salt of any one of Claims 147 to 155, wherein the choline salt of the compound is characterized by an x-ray powder diffraction substantially similar to FIGURE 15A. 157. The choline salt of any one of Claims 147 to 156, wherein the choline salt of the compound is further characterized by a differential scanning calorimeter (DSC) thermogram comprising a peak endotherm at 172.1 °C ± 2 °C. 158. The choline salt of any one of Claims 147 to 157, wherein the molar ratio of choline counter-ion to compound is about 1.0. 159. The choline salt of any one of Claims 147 to 158, wherein the choline salt of the compound is an anhydrate. 160. The choline salt of Claim 147 or 148, wherein the choline salt of the compound is crystalline Form II characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 6.6°, 9.9°, 10.9°, 13.3°, 20.0°, 21.4°, and 23.4°. 136 ME1\53438692.v1 136867-00920 161. The choline salt of any one of Claims 147, 148, and 160, wherein the choline salt of the compound is crystalline Form II characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 6.6°, 9.9°, 10.9°, 13.3°, 20.0°, 21.4°, and 23.4°. 162. The choline salt of any one of Claims 147, 148, 160, and 161, wherein the choline salt of the compound is crystalline Form II characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 6.6°, 9.9°, 10.9°, 13.3°, 20.0°, 21.4°, and 23.4°. 163. The choline salt of any one of Claims 147, 148, and 160 to 162, wherein the choline salt of the compound is crystalline Form II characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 6.6°, 9.9°, 10.9°, 13.3°, 20.0°, 21.4°, and 23.4°. 164. The choline salt of any one of Claims 147, 148, and 160 to 163, wherein the choline salt of the compound is crystalline Form II characterized by x-ray powder diffraction peaks at 2θ angles 6.6°, 9.9°, 10.9°, 13.3°, 20.0°, 21.4°, and 23.4°. 165. The choline salt of any one of Claims 147, 148, and 160 to 164, wherein the choline salt of the compound is crystalline Form II further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 11.7°, 21.8°, 23.4°, and 27.5°. 166. The choline salt of any one of Claims 147, 148, and 160 to 165, wherein the choline salt of the compound is characterized by an x-ray powder diffraction substantially similar to FIGURE 16. 167. The choline salt of Claim 147 or 148, wherein the choline salt of the compound is crystalline Form III characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 7.4°, 11.1°, 14.8°, and 22.3°. 168. The choline salt of any one of Claims 147, 148, and 167, wherein the choline salt of the compound is crystalline Form III characterized by x-ray powder diffraction peaks at 2θ angles 7.4°, 11.1°, 14.8°, and 22.3°. 137 ME1\53438692.v1 136867-00920 169. The choline salt of any one of Claims 147, 148, 167, and 168, wherein the choline salt of the compound is crystalline Form III further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 16.5°, 18.6°, 20.3°, and 33.4°. 170. The choline salt of any one of Claims 147, 148, and 167 to 169, wherein the choline salt of the compound is characterized by an x-ray powder diffraction substantially similar to FIGURE 17A. 171. The choline salt of any one of Claims 147, 148, and 167 to 170, wherein the choline salt of the compound is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 131.8 °C, and 175.7 °C, and a peak exotherm at 135.3 °C ± 2 °C. 172. The choline salt of any one of Claims 147, 148, and 167 to 171, wherein the molar ratio of choline counter-ion to compound is about 1.1. 173. The choline salt of any one of Claims 147, 148, and 167 to 172, wherein the choline salt of the compound is an anhydrate. 174. The choline salt of Claim 147 or 148, wherein the choline salt of the compound is crystalline Form IV characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 10.5°, 13.3°, 17.4°, 18.3°, 20.7°, and 23.8°. 175. The choline salt of any one of Claims 147, 148, and 174, wherein the choline salt of the compound is crystalline Form IV characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 10.5°, 13.3°, 17.4°, 18.3°, 20.7°, and 23.8°. 176. The choline salt of any one of Claims 147, 148, 174, and 175, wherein the choline salt of the compound is crystalline Form IV characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 10.5°, 13.3°, 17.4°, 18.3°, 20.7°, and 23.8°. 138 ME1\53438692.v1 136867-00920 177. The choline salt of any one of Claims 147, 148, and 174 to 176, wherein the choline salt of the compound is crystalline Form IV characterized by x-ray powder diffraction peaks at 2θ angles 10.5°, 13.3°, 17.4°, 18.3°, 20.7°, and 23.8°. 178. The choline salt of any one of Claims 147, 148, and 174 to 177, wherein the choline salt of the compound is crystalline Form IV further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 11.3°, 17.8°, 18.9°, 21.1°, 22.3°, 23.4°, and 24.3°. 179. The choline salt of any one of Claims 147, 148, and 174 to 178, wherein the choline salt of the compound is characterized by an x-ray powder diffraction substantially similar to FIGURE 18A. 180. The choline salt of any one of Claims 147, 148, and 174 to 179, wherein the choline salt of the compound is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 116.4 °C, 142.3 °C, and 176.2 °C, and a peak exotherm at 144.6 °C ± 2 °C. 181. The choline salt of any one of Claims 147, 148, and 174 to 180, wherein the molar ratio of choline counter-ion to compound is about 1.1. 182. The choline salt of any one of Claims 147, 148, and 174 to 181, wherein the choline salt of the compound is an EtOH solvate. 183. The choline salt of Claim 147 or 148, wherein the choline salt of the compound is crystalline Form V characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 10.6°, 14.5°, 17.4°, 18.6°, 20.7°, and 21.2°. 184. The choline salt of any one of Claims 147, 148 and 183, wherein the choline salt of the compound is crystalline Form V characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 10.6°, 14.5°, 17.4°, 18.6°, 20.7°, and 21.2°. 139 ME1\53438692.v1 136867-00920 185. The choline salt of any one of Claims 147, 148, 183 and 184, wherein the choline salt of the compound is crystalline Form V characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 10.6°, 14.5°, 17.4°, 18.6°, 20.7°, and 21.2°. 186. The choline salt of any one of Claims 147, 148, and 183 to 185, wherein the choline salt of the compound is crystalline Form V characterized by x-ray powder diffraction peaks at 2θ angles 10.6°, 14.5°, 17.4°, 18.6°, 20.7°, and 21.2°. 187. The choline salt of any one of Claims 147, 148, and 183 to 186, wherein the choline salt of the compound is crystalline Form V further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 11.4°, 15.6°, 17.8°, 19.8°, and 24.2°. 188. The choline salt of any one of Claims 147, 148, and 183 to 187, wherein the choline salt of the compound is characterized by an x-ray powder diffraction substantially similar to FIGURE 19A. 189. The choline salt of any one of Claims 147, 148, and 183 to 188, wherein the choline salt of the compound is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 142.2 °C, and 176.3 °C, and a peak exotherm at 144.8 °C ± 2 °C. 190. The choline salt of any one of Claims 147, 148, and 183 to 189, wherein the molar ratio of choline counter-ion to compound is about 1.1. 191. The choline salt of any one of Claims 147, 148, and 183 to 190, wherein the choline salt of the compound is an anhydrate. 192. The choline salt of Claim 147 or 148, wherein the choline salt of the compound is crystalline Form VI characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 11.2°, 16.4°, 17.0°, 19.3°, 20.0°, 20.4°, and 22.9°. 140 ME1\53438692.v1 136867-00920 193. The choline salt of any one of Claims 147, 148, and 192, wherein the choline salt of the compound is crystalline Form VI characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 11.2°, 16.4°, 17.0°, 19.3°, 20.0°, 20.4°, and 22.9°. 194. The choline salt of any one of Claims 147, 148, 192, and 193, wherein the choline salt of the compound is crystalline Form VI characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 11.2°, 16.4°, 17.0°, 19.3°, 20.0°, 20.4°, and 22.9°. 195. The choline salt of any one of Claims 147, 148, and 192 to 194, wherein the choline salt of the compound is crystalline Form VI characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 11.2°, 16.4°, 17.0°, 19.3°, 20.0°, 20.4°, and 22.9°. 196. The choline salt of any one of Claims 147, 148, and 192 to 195, wherein the choline salt of the compound is crystalline Form VI characterized by x-ray powder diffraction peaks at 2θ angles 11.2°, 16.4°, 17.0°, 19.3°, 20.0°, 20.4°, and 22.9°. 197. The choline salt of any one of Claims 147, 148, and 192 to 196, wherein the choline salt of the compound is crystalline Form VI further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 14.1°, 14.4°, 16.1°, 16.7°, 18.9°, 21.1°, and 22.4°. 198. The choline salt of any one of Claims 147, 148, and 192 to 197, wherein the choline salt of the compound is characterized by an x-ray powder diffraction substantially similar to FIGURE 20A. 199. The choline salt of any one of Claims 147, 148, and 192 to 198, wherein the choline salt of the compound is further characterized by a differential scanning calorimeter (DSC) thermogram comprising a peak endotherm at 174.6 °C ± 2 °C. 200. The choline salt of any one of Claims 147, 148, and 192 to 199, wherein the molar ratio of choline counter-ion to compound is about 1.1. 141 ME1\53438692.v1 136867-00920 201. The choline salt of any one of Claims 147, 148, and 192 to 200, wherein the choline salt of the compound is an anhydrate. 202. A hydrogen bromide salt of the compound 3-[[3-fluoro-2-(methylsulfamoylamino)-4- pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one. 203. The hydrogen bromide salt of Claim 202, wherein the hydrogen bromide salt is crystalline. 204. The hydrogen bromide salt of Claim 202 or 203, wherein the hydrogen bromide salt of the compound is crystalline Form I characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 4.8°, 8.7°, 15.2°, 17.7°, 24.1°, and 30.0°. 205. The hydrogen bromide salt of any one of Claims 202 to 204, wherein the hydrogen bromide salt of the compound is crystalline Form I characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 4.8°, 8.7°, 15.2°, 17.7°, 24.1°, and 30.0°. 206. The hydrogen bromide salt of any one of Claims 202 to 205, wherein the hydrogen bromide salt of the compound is crystalline Form I characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 4.8°, 8.7°, 15.2°, 17.7°, 24.1°, and 30.0°. 207. The hydrogen bromide salt of any one of Claims 202 to 206, wherein the hydrogen bromide salt of the compound is crystalline Form I characterized by x-ray powder diffraction peaks at 2θ angles 4.8°, 8.7°, 15.2°, 17.7°, 24.1°, and 30.0°. 208. The hydrogen bromide salt of any one of Claims 202 to 207, wherein the hydrogen bromide salt of the compound is crystalline Form I further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 13.2°, 14.5°, 14.9°, and 15.8°. 209. The hydrogen bromide salt of any one of Claims 202 to 208, wherein the hydrogen bromide salt of the compound is characterized by an x-ray powder diffraction substantially similar to FIGURE 21A. 142 ME1\53438692.v1 136867-00920 210. The hydrogen bromide salt of any one of Claims 202 to 209, wherein the hydrogen bromide salt of the compound is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 81.9 °C, 116.7 °C, 146.8 °C, and 169.7 °C ± 2 °C. 211. The hydrogen bromide salt of any one of Claims 202 to 210, wherein the molar ratio of bromide counter-ion to compound is about 0.7. 212. The hydrogen bromide salt of Claim 202 or 203, wherein the hydrogen bromide salt of the compound is crystalline Form II characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 4.9°, 10.8°, 14.5°, 15.3°, 19.4°, 23.6°, and 24.2°. 213. The hydrogen bromide salt of any one of Claims 202, 203, and 212, wherein the hydrogen bromide salt of the compound is crystalline Form II characterized by at least four x- ray powder diffraction peaks at 2θ angles selected from 4.9°, 10.8°, 14.5°, 15.3°, 19.4°, 23.6°, and 24.2°. 214. The hydrogen bromide salt of any one of Claims 202, 203, 212, and 213, wherein the hydrogen bromide salt of the compound is crystalline Form II characterized by at least five x- ray powder diffraction peaks at 2θ angles selected from 4.9°, 10.8°, 14.5°, 15.3°, 19.4°, 23.6°, and 24.2°. 215. The hydrogen bromide salt of any one of Claims 202, 203, and 212 to 214, wherein the hydrogen bromide salt of the compound is crystalline Form II characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 4.9°, 10.8°, 14.5°, 15.3°, 19.4°, 23.6°, and 24.2°. 216. The hydrogen bromide salt of any one of Claims 202, 203, and 212 to 215, wherein the hydrogen bromide salt of the compound is crystalline Form II characterized by x-ray powder diffraction peaks at 2θ angles 4.9°, 10.8°, 14.5°, 15.3°, 19.4°, 23.6°, and 24.2°. 217. The hydrogen bromide salt of any one of Claims 202, 203, and 212 to 216, wherein the hydrogen bromide salt of the compound is crystalline Form II further characterized by 143 ME1\53438692.v1 136867-00920 one or more x-ray powder diffraction peaks at 2θ angles selected from 6.8°, 9.7°, 15.6°, 17.4°, 21.6°, 29.2°, and 30.8°. 218. The hydrogen bromide salt of any one of Claims 202, 203, and 212 to 217, wherein the hydrogen bromide salt of the compound is characterized by an x-ray powder diffraction substantially similar to FIGURE 22A. 219. The hydrogen bromide salt of any one of Claims 202, 203, and 212 to 218, wherein the hydrogen bromide salt of the compound is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 111.2 °C and 147.8 °C ± 2 °C. 220. The hydrogen bromide salt of any one of Claims 202, 203, and 212 to 219, wherein the molar ratio of bromide counter-ion to compound is about 1.0. 221. The hydrogen bromide salt of any one of Claims 202, 203, and 212 to 220, wherein the hydrogen bromide salt of the compound is a hydrate. 222. The hydrogen bromide salt of Claim 202 or 203, wherein the hydrogen bromide salt of the compound is crystalline Form III characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 5.2°, 8.0°, 13.1°, 15.6°, 17.6°, 22.4°, and 28.9°. 223. The hydrogen bromide salt of any one of Claims 202, 203, and 222, wherein the hydrogen bromide salt of the compound is crystalline Form III characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 5.2°, 8.0°, 13.1°, 15.6°, 17.6°, 22.4°, and 28.9°. 224. The hydrogen bromide salt of any one of Claims 202, 203, 222, and 223, wherein the hydrogen bromide salt of the compound is crystalline Form III characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 5.2°, 8.0°, 13.1°, 15.6°, 17.6°, 22.4°, and 28.9°. 144 ME1\53438692.v1 136867-00920 225. The hydrogen bromide salt of Claim 202, 203, and 222 to 224, wherein the hydrogen bromide salt of the compound is crystalline Form III characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 5.2°, 8.0°, 13.1°, 15.6°, 17.6°, 22.4°, and 28.9°. 226. The hydrogen bromide salt of any one of Claims 202, 203, and 222 to 225, wherein the hydrogen bromide salt of the compound is crystalline Form III characterized by x-ray powder diffraction peaks at 2θ angles 5.2°, 8.0°, 13.1°, 15.6°, 17.6°, 22.4°, and 28.9°. 227. The hydrogen bromide salt of any one of Claims 202, 203, and 222 to 226, wherein the hydrogen bromide salt of the compound is crystalline Form III further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 6.6°, 15.0°, 16.1°, 19.2°, 20.8°, and 21.1°. 228. The hydrogen bromide salt of any one of Claims 202, 203, and 222 to 227, wherein the hydrogen bromide salt of the compound is characterized by an x-ray powder diffraction substantially similar to FIGURE 23A. 228. A 1,5-naphthalenedisulfonate salt of the compound 3-[[3-fluoro-2- (methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen- 2-one. 229. The 1,5-naphthalenedisulfonate salt of Claim 228, wherein the 1,5- naphthalenedisulfonate salt is crystalline. 230. The 1,5-naphthalenedisulfonate salt of Claim 228 or 229, wherein the 1,5- naphthalenedisulfonate salt of the compound is crystalline Form I characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 8.3°, 11.1°, 12.2°, 14.0°, 15.7°, and 16.0°. 231. The 1,5-naphthalenedisulfonate salt of any one of Claims 228 to 230, wherein the 1,5- naphthalenedisulfonate salt of the compound is crystalline Form I characterized by at least 145 ME1\53438692.v1 136867-00920 four x-ray powder diffraction peaks at 2θ angles selected from 8.3°, 11.1°, 12.2°, 14.0°, 15.7°, and 16.0°. 232. The 1,5-naphthalenedisulfonate salt of any one of Claims 228 to 231, wherein the 1,5- naphthalenedisulfonate salt of the compound is crystalline Form I characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 8.3°, 11.1°, 12.2°, 14.0°, 15.7°, and 16.0°. 233. The 1,5-naphthalenedisulfonate salt of any one of Claims 228 to 232, wherein the 1,5- naphthalenedisulfonate salt of the compound is crystalline Form I characterized by x-ray powder diffraction peaks at 2θ angles 8.3°, 11.1°, 12.2°, 14.0°, 15.7°, and 16.0°. 234. The 1,5-naphthalenedisulfonate salt of any one of Claims 228 to 233, wherein the 1,5- naphthalenedisulfonate salt of the compound is crystalline Form I further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 7.5°, 13.1°, 14.5°, 15.0°, 16.4°, 16.7°, and 16.9°. 235. The 1,5-naphthalenedisulfonate salt of any one of Claims 228 to 234, wherein the 1,5- naphthalenedisulfonate salt of the compound is characterized by an x-ray powder diffraction substantially similar to FIGURE 24A. 236. The 1,5-naphthalenedisulfonate salt of any one of Claims 228 to 235, wherein the 1,5- naphthalenedisulfonate salt of the compound is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 110.2 °C and 185.0 °C ± 2 °C. 237. The 1,5-naphthalenedisulfonate salt of any one of Claims 228 to 236, wherein the molar ratio of 1,5-naphthalenedisulfonate counter-ion to compound is about 0.7. 238. The 1,5-naphthalenedisulfonate salt of Claim 228 or 229, wherein the 1,5- naphthalenedisulfonate salt of the compound is crystalline Form II characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 5.9°, 13.2°, 18.2°, 18.6°, 23.2°, 25.8°, and 26.3°. 146 ME1\53438692.v1 136867-00920 239. The 1,5-naphthalenedisulfonate salt of any one of Claims 228, 229, and 238, wherein the 1,5-naphthalenedisulfonate salt of the compound is crystalline Form II characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 5.9°, 13.2°, 18.2°, 18.6°, 23.2°, 25.8°, and 26.3°. 240. The 1,5-naphthalenedisulfonate salt of any one of Claims 228, 229, 238, and 239, wherein the 1,5-naphthalenedisulfonate salt of the compound is crystalline Form II characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 5.9°, 13.2°, 18.2°, 18.6°, 23.2°, 25.8°, and 26.3°. 241. The 1,5-naphthalenedisulfonate salt of any one of Claims 228, 229, and 238 to 240, wherein the 1,5-naphthalenedisulfonate salt of the compound is crystalline Form II characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 5.9°, 13.2°, 18.2°, 18.6°, 23.2°, 25.8°, and 26.3°. 242. The 1,5-naphthalenedisulfonate salt of any one of Claims 228, 229, and 238 to 241, wherein the 1,5-naphthalenedisulfonate salt of the compound is crystalline Form II characterized by x-ray powder diffraction peaks at 2θ angles 5.9°, 13.2°, 18.2°, 18.6°, 23.2°, 25.8°, and 26.3°. 243. The 1,5-naphthalenedisulfonate salt of any one of Claims 228, 229, and 238 to 242, wherein the 1,5-naphthalenedisulfonate salt of the compound is crystalline Form II further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 7.5°, 14.1°, 15.7°, and 22.5°. 244. The 1,5-naphthalenedisulfonate salt of any one of Claims 228, 229, and 238 to 243, wherein the 1,5-naphthalenedisulfonate salt of the compound is characterized by an x-ray powder diffraction substantially similar to FIGURE 25A. 245. The 1,5-naphthalenedisulfonate salt of any one of Claims 228, 229, and 238 to 244, wherein the 1,5-naphthalenedisulfonate salt of the compound is further characterized by a 147 ME1\53438692.v1 136867-00920 differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 130.9 ºC, 155.2 ºC and 164.3 ºC and a peak exotherm at 143.7 ºC ± 2 °C. 246. The 1,5-naphthalenedisulfonate salt of any one of Claims 228, 229, and 238 to 245, wherein the molar ratio of 1,5-naphthalenedisulfonate counter-ion to compound is about 0.9. 247. An edisylate salt of the compound 3-[[3-fluoro-2-(methylsulfamoylamino)-4- pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one. 248. The edisylate salt of Claim 247, wherein the edisylate salt of the compound is crystalline. 249. The edisylate salt of Claim 247 or 248, wherein the edisylate salt of the compound is crystalline Form I characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 13.3°, 14.3°, 14.8°, and 19.1°. 250. The edisylate salt of any one of Claims 247 to 249, wherein the edisylate salt of the compound is crystalline Form I characterized by x-ray powder diffraction peaks at 2θ angles 13.3°, 14.3°, 14.8°, and 19.1°. 251. The edisylate salt of any one of Claims 247 to 250, wherein the edisylate salt of the compound is crystalline Form I further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 9.6°, 12.6°, 15.5°, and 17.3°. 252. The edisylate salt of any one of Claims 247 to 251, wherein the edisylate salt of the compound is characterized by an x-ray powder diffraction substantially similar to FIGURE 26A. 253. The edisylate salt of any one of Claims 247 to 252, wherein the edisylate salt of the compound is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 80.1 °C, 156.8 °C, and 170.5 °C ± 2 °C. 148 ME1\53438692.v1 136867-00920 254. The edisylate salt of any one of Claims 247 to 253, wherein the molar ratio of edisylate counter-ion to compound is about 0.8. 255. The edisylate salt of Claim 247 or 248, wherein the edisylate salt of the compound is crystalline Form II characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 6.0°, 16.6°, 17.2°, 18.2°, 21.3°, 21.7°, and 22.4°. 256. The edisylate salt of any one of Claims 247, 248, and 255, wherein the edisylate salt of the compound is crystalline Form II characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 6.0°, 16.6°, 17.2°, 18.2°, 21.3°, 21.7°, and 22.4°. 257. The edisylate of any one of Claims 247, 248, 255, and 256, wherein the edisylate salt of the compound is crystalline Form II characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 6.0°, 16.6°, 17.2°, 18.2°, 21.3°, 21.7°, and 22.4°. 258. The edisylate salt of any one of Claims 247, 248, and 255 to 257, wherein the edisylate salt of the compound is crystalline Form II characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 6.0°, 16.6°, 17.2°, 18.2°, 21.3°, 21.7°, and 22.4°. 259. The edisylate salt of any one of Claims 247, 248, and 255 to 258, wherein the edisylate salt of the compound is crystalline Form II characterized by x-ray powder diffraction peaks at 2θ angles 6.0°, 16.6°, 17.2°, 18.2°, 21.3°, 21.7°, and 22.4°. 260. The edisylate salt of any one of Claims 247, 248, and 255 to 259, wherein the edisylate salt of the compound is crystalline Form II further characterized by one or more x- ray powder diffraction peaks at 2θ angles selected from 13.5°, 17.5°, 19.1°, and 23.0°. 261. The edisylate salt of any one of Claims 247, 248, and 255 to 260, wherein the edisylate salt of the compound is characterized by an x-ray powder diffraction substantially similar to FIGURE 27A. 149 ME1\53438692.v1 136867-00920 262. The edisylate salt of any one of Claims 247, 248, and 255 to 261, wherein the edisylate salt of the compound is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 74.2 ºC, 116.5 ºC and 131.1 ºC and a peak exotherm at 143.7 ºC ± 2 °C. 263. The edisylate salt of any one of Claims 247, 248, and 255 to 262, wherein the molar ratio of edisylate counter-ion to compound is about 0.8. 264. A diethylamine salt of the compound 3-[[3-fluoro-2-(methylsulfamoylamino)-4- pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one. 265. The diethylamine salt of Claim 264, wherein the diethylamine salt of the compound is crystalline. 266. The diethylamine salt of Claim 264 or 265, wherein the diethylamine salt of the compound is crystalline Form I characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 12.9°, 13.4°, 17.7°, 19.0°, 21.4°, 25.0°, and 30.0°. 267. The diethylamine salt of any one of Claims 264 to 266, wherein the diethylamine salt of the compound is crystalline Form I characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 12.9°, 13.4°, 17.7°, 19.0°, 21.4°, 25.0°, and 30.0°. 268. The diethylamine salt of any one of Claims 264 to 267, wherein the diethylamine salt of the compound is crystalline Form I characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 12.9°, 13.4°, 17.7°, 19.0°, 21.4°, 25.0°, and 30.0°. 269. The diethylamine salt of any one of Claims 264 to 268, wherein the diethylamine salt of the compound is crystalline Form I characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 12.9°, 13.4°, 17.7°, 19.0°, 21.4°, 25.0°, and 30.0°. 270. The diethylamine salt of any one of Claims 264 to 269, wherein the diethylamine salt of the compound is crystalline Form I characterized by x-ray powder diffraction peaks at 2θ angles 12.9°, 13.4°, 17.7°, 19.0°, 21.4°, 25.0°, and 30.0°. 150 ME1\53438692.v1 136867-00920 271. The diethylamine salt of any one of Claims 264 to 270, wherein the diethylamine salt of the compound is crystalline Form I further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 8.7°, 13.2°, 14.9°, 15.1°, 15.8°, 17.0°, 20.3°, 21.1°, and 23.4°. 272. The diethylamine salt of any one of Claims 264 to 271, wherein the diethylamine salt of the compound is characterized by an x-ray powder diffraction substantially similar to FIGURE 28A. 273. The diethylamine salt of any one of Claims 264 to 272, wherein the diethylamine salt of the compound is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 98.7 °C and 195.9 °C ± 2 °C. 274. The diethylamine salt of any one of Claims 264 to 273, wherein the molar ratio of diethylamine counter-ion to compound is about 0.5. 275. The diethylamine salt of Claim 264 or 265, wherein the diethylamine salt of the compound is crystalline Form II characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 3.7°, 7.3°, 11.0°, 12.3°, 13.8°, 14.6°, 16.9°, and 17.9°. 276. The diethylamine salt of any one of Claims 264, 265, and 275, wherein the diethylamine salt of the compound is crystalline Form II characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 3.7°, 7.3°, 11.0°, 12.3°, 13.8°, 14.6°, 16.9°, and 17.9°. 277. The diethylamine salt of any one of Claims 264, 265, 275, and 276, wherein the diethylamine salt of the compound is crystalline Form II characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 3.7°, 7.3°, 11.0°, 12.3°, 13.8°, 14.6°, 16.9°, and 17.9°. 278. The diethylamine salt of any one of Claims 264, 265, and 275 to 277, wherein the diethylamine salt of the compound is crystalline Form II characterized by at least six x-ray 151 ME1\53438692.v1 136867-00920 powder diffraction peaks at 2θ angles selected from 3.7°, 7.3°, 11.0°, 12.3°, 13.8°, 14.6°, 16.9°, and 17.9°. 279. The diethylamine salt of any one of Claims 264, 265, and 275 to 278, wherein the diethylamine salt of the compound is crystalline Form II characterized by at least seven x-ray powder diffraction peaks at 2θ angles selected from 3.7°, 7.3°, 11.0°, 12.3°, 13.8°, 14.6°, 16.9°, and 17.9°. 280. The diethylamine salt of any one of Claims 264, 265, and 275 to 279, wherein the diethylamine salt of the compound is crystalline Form II characterized by x-ray powder diffraction peaks at 2θ angles 3.7°, 7.3°, 11.0°, 12.3°, 13.8°, 14.6°, 16.9°, and 17.9°. 281. The diethylamine salt of any one of Claims 264, 265, and 275 to 280, wherein the diethylamine salt of the compound is crystalline Form II further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 8.5°, 10.3°, 18.2°, 20.9°, and 22.9°. 282. The diethylamine salt of any one of Claims 264, 265, and 275 to 281, wherein the diethylamine salt of the compound is characterized by an x-ray powder diffraction substantially similar to FIGURE 29A. 283. The diethylamine salt of any one of Claims 264, 265, and 275 to 282, wherein the diethylamine salt of the compound is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 119.8 ºC, 180.0 ºC and 192.0 ºC. 284. The diethylamine salt of any one of Claims 264, 265, and 275 to 283, wherein the molar ratio of diethylamine counter-ion to compound is about 0.9. 285. A hydrogen chloride salt of the compound 3-[[3-fluoro-2-(methylsulfamoylamino)-4- pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one. 286. The hydrogen chloride salt of Claim 285, wherein the hydrogen chloride salt is crystalline. 152 ME1\53438692.v1 136867-00920 287. The hydrogen chloride salt of Claim 285 or 286, wherein the hydrogen chloride salt of the compound is crystalline Form I characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 4.8°, 6.8°, 14.4°, 15.3°, 19.4°, and 24.1°. 288. The hydrogen chloride salt of any one of Claims 285 to 287, wherein the hydrogen chloride salt of the compound is crystalline Form I characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 4.8°, 6.8°, 14.4°, 15.3°, 19.4°, and 24.1°. 289. The hydrogen chloride salt of any one of Claims 285 to 288, wherein the hydrogen chloride salt of the compound is crystalline Form I characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 4.8°, 6.8°, 14.4°, 15.3°, 19.4°, and 24.1°. 290. The hydrogen chloride salt of any one of Claims 285 to 289, wherein the hydrogen chloride salt of the compound is crystalline Form I characterized by x-ray powder diffraction peaks at 2θ angles 4.8°, 6.8°, 14.4°, 15.3°, 19.4°, and 24.1°. 291. The hydrogen chloride salt of any one of Claims 285 to 290, wherein the hydrogen chloride salt of the compound is crystalline Form I further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 9.7°, 15.9°, 21.7°, 29.2°, and 30.9°. 292. The hydrogen chloride salt of any one of Claims 285 to 291, wherein the hydrogen chloride salt of the compound is characterized by an x-ray powder diffraction substantially similar to FIGURE 30A. 293. The hydrogen chloride salt of any one of Claims 285 to 292, wherein the hydrogen chloride salt of the compound is further characterized by a differential scanning calorimeter (DSC) thermogram comprising peak endotherms at 93.9 ºC, 137.6 ºC, 153.4 ºC, and 166.7 ºC ± 2 °C. 294. The hydrogen chloride salt of any one of Claims 285 to 293, wherein the molar ratio of chloride counter-ion to compound is about 0.6. 153 ME1\53438692.v1 136867-00920 295. The hydrogen chloride salt of Claim 285 or 286, wherein the hydrogen chloride salt of the compound is crystalline Form II characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 4.8°, 8.7°, 13.3°, 17.8°, 24.1°, 29.0°, and 30.0°. 296. The hydrogen chloride salt of any one of Claims 285, 286, and 295, wherein the hydrogen chloride salt of the compound is crystalline Form II characterized by at least four x- ray powder diffraction peaks at 2θ angles selected from 4.8°, 8.7°, 13.3°, 17.8°, 24.1°, 29.0°, and 30.0°. 297. The hydrogen chloride salt of any one of Claims 285, 286, 295, and 296, wherein the hydrogen chloride salt of the compound is crystalline Form II characterized by at least five x- ray powder diffraction peaks at 2θ angles selected from 4.8°, 8.7°, 13.3°, 17.8°, 24.1°, 29.0°, and 30.0°. 298. The hydrogen chloride salt of any one of Claims 285, 286, and 295 to 297, wherein the hydrogen chloride salt of the compound is crystalline Form II characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 4.8°, 8.7°, 13.3°, 17.8°, 24.1°, 29.0°, and 30.0°. 299. The hydrogen chloride salt of any one of Claims 285, 286, and 295 to 298, wherein the hydrogen chloride salt of the compound is crystalline Form II characterized by x-ray powder diffraction peaks at 2θ angles 4.8°, 8.7°, 13.3°, 17.8°, 24.1°, 29.0°, and 30.0°. 300. The hydrogen chloride salt of any one of Claims 285, 286, and 295 to 299, wherein the hydrogen chloride salt of the compound is crystalline Form II further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 5.4°, 9.6°, 12.4°, 14.4°, 19.2°, and 33.9°. 301. The hydrogen chloride salt of any one of Claims 285, 286, and 295 to 300, wherein the hydrogen chloride salt of the compound is characterized by an x-ray powder diffraction substantially similar to FIGURE 31. 154 ME1\53438692.v1 136867-00920 302. The hydrogen chloride salt of Claim 285 or 286, wherein the hydrogen chloride salt of the compound is crystalline Form III characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 4.8°, 6.3°, 8.7°, 14.2°, 16.5°, 23.5°, and 24.1°. 303. The hydrogen chloride salt of any one of Claims 285, 286, and 302, wherein the hydrogen chloride salt of the compound is crystalline Form III characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 4.8°, 6.3°, 8.7°, 14.2°, 16.5°, 23.5°, and 24.1°. 304. The hydrogen chloride salt of any one of Claims 285, 286, 302, and 303, wherein the hydrogen chloride salt of the compound is crystalline Form III characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 4.8°, 6.3°, 8.7°, 14.2°, 16.5°, 23.5°, and 24.1°. 305. The hydrogen chloride salt of any one of Claims 285, 286, and 302 to 304, wherein the hydrogen chloride salt of the compound is crystalline Form III characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 4.8°, 6.3°, 8.7°, 14.2°, 16.5°, 23.5°, and 24.1°. 306. The hydrogen chloride salt of any one of Claims 285, 286, and 302 to 305, wherein the hydrogen chloride salt of the compound is crystalline Form III characterized by x-ray powder diffraction peaks at 2θ angles 4.8°, 6.3°, 8.7°, 14.2°, 16.5°, 23.5°, and 24.1°. 307. The hydrogen chloride salt of any one of Claims 285, 286, and 302 to 306, wherein the hydrogen chloride salt of the compound is crystalline Form III further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 8.1°, 19.2°, 20.3°, 25.1°, and 30.0°. 308. The hydrogen chloride salt of any one of Claims 285, 286, and 302 to 307, wherein the hydrogen chloride salt of the compound is characterized by an x-ray powder diffraction substantially similar to FIGURE 32. 155 ME1\53438692.v1 136867-00920 309. The hydrogen chloride salt of Claim 285 or 286, wherein the hydrogen chloride salt of the compound is crystalline Form IV characterized by at least three x-ray powder diffraction peaks at 2θ angles selected from 4.8°, 8.7°, 13.2°, 13.3°, 15.8°, 17.7°, 21.1°, and 30.0°. 310. The hydrogen chloride salt of any one of Claims 285, 286, and 309, wherein the hydrogen chloride salt of the compound is crystalline Form IV characterized by at least four x-ray powder diffraction peaks at 2θ angles selected from 4.8°, 8.7°, 13.2°, 13.3°, 15.8°, 17.7°, 21.1°, and 30.0°. 311. The hydrogen chloride salt of any one of Claims 285, 286, 309, and 310, wherein the hydrogen chloride salt of the compound is crystalline Form IV characterized by at least five x-ray powder diffraction peaks at 2θ angles selected from 4.8°, 8.7°, 13.2°, 13.3°, 15.8°, 17.7°, 21.1°, and 30.0°. 312. The hydrogen chloride salt of any one of Claims 285, 286, and 309 to 311, wherein the hydrogen chloride salt of the compound is crystalline Form IV characterized by at least six x-ray powder diffraction peaks at 2θ angles selected from 4.8°, 8.7°, 13.2°, 13.3°, 15.8°, 17.7°, 21.1°, and 30.0°. 313. The hydrogen chloride salt of any one of Claims 285, 286, and 309 to 312, wherein the hydrogen chloride salt of the compound is crystalline Form IV characterized by at least seven x-ray powder diffraction peaks at 2θ angles selected from 4.8°, 8.7°, 13.2°, 13.3°, 15.8°, 17.7°, 21.1°, and 30.0°. 314. The hydrogen chloride salt of any one of Claims 285, 286, and 309 to 313, wherein the hydrogen chloride salt of the compound is crystalline Form IV characterized by x-ray powder diffraction peaks at 2θ angles 4.8°, 8.7°, 13.2°, 13.3°, 15.8°, 17.7°, 21.1°, and 30.0°. 315. The hydrogen chloride salt of any one of Claims 285, 286, and 309 to 314, wherein the hydrogen chloride salt of the compound is crystalline Form IV further characterized by one or more x-ray powder diffraction peaks at 2θ angles selected from 5.4°, 14.2°, 14.9°, 16.2°, 17.4° and 19.6°. 156 ME1\53438692.v1 136867-00920 316. The hydrogen chloride salt of any one of Claims 285, 286, and 309 to 315, wherein the hydrogen chloride salt of the compound is characterized by an x-ray powder diffraction substantially similar to FIGURE 33A. 317. The hydrogen chloride salt of any one of Claims 285, 286, and 309 to 316, wherein the hydrogen chloride salt of the compound is further characterized by a differential scanning calorimeter (DSC) thermogram comprising a peak endotherm at 178.5 ºC, and peak exotherms at 91.6 ºC and 160.2 ºC. 318. The hydrogen chloride salt of any one of Claims 285, 286, and 309 to 317, wherein the molar ratio of chloride counter-ion to compound is about 0.3. 319. A pharmaceutical composition comprising the crystalline salt of any one of claims 1- 318, and a pharmaceutically acceptable carrier. 320. A method of inhibiting mitogen-activated protein kinase (MEK) in a subject in need thereof, comprising administering to the subject a therapeutically effective amount of the salt of any one of claims 1-318, and/or the composition of claim 319. 321. A method of treating a disease responsive to the inhibition of mitogen-activated protein kinase (MEK) in a subject in need thereof, comprising administering to the subject a therapeutically effective amount of the salt of any one of claims 1-318, or the composition of claim 319. 322. The method of claim 321, wherein the disease is cancer. 157 ME1\53438692.v1
PCT/US2025/033293 2024-06-13 2025-06-12 Crystalline forms of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]jmethyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one Pending WO2025259841A1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US202463659793P 2024-06-13 2024-06-13
US63/659,793 2024-06-13

Publications (1)

Publication Number Publication Date
WO2025259841A1 true WO2025259841A1 (en) 2025-12-18

Family

ID=96500161

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/US2025/033293 Pending WO2025259841A1 (en) 2024-06-13 2025-06-12 Crystalline forms of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]jmethyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one

Country Status (1)

Country Link
WO (1) WO2025259841A1 (en)

Citations (23)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US510A (en) 1837-12-07 soeel
US949A (en) 1838-09-27 Improvement in roller cotton-gins for ginning long-staple and other kinds of cotton
US5863A (en) 1848-10-17 Matthias p
US5861A (en) 1848-10-17 Locking umbrella and parasol
WO1990005719A1 (en) 1988-11-23 1990-05-31 British Bio-Technology Limited Hydroxamic acid based collagenase inhibitors
EP0606046A1 (en) 1993-01-06 1994-07-13 Ciba-Geigy Ag Arylsulfonamido-substituted hydroxamic acids
WO1996027583A1 (en) 1995-03-08 1996-09-12 Pfizer Inc. Arylsulfonylamino hydroxamic acid derivatives
WO1996033172A1 (en) 1995-04-20 1996-10-24 Pfizer Inc. Arylsulfonyl hydroxamic acid derivatives as mmp and tnf inhibitors
EP0780386A1 (en) 1995-12-20 1997-06-25 F. Hoffmann-La Roche Ag Matrix metalloprotease inhibitors
WO1998001113A1 (en) 1996-07-04 1998-01-15 Seiken Chemical Co., Ltd. Lubrication assistant and process for the preparation of ethyl stearate used therein
WO1998003516A1 (en) 1996-07-18 1998-01-29 Pfizer Inc. Phosphinate based inhibitors of matrix metalloproteases
WO1998007697A1 (en) 1996-08-23 1998-02-26 Pfizer Inc. Arylsulfonylamino hydroxamic acid derivatives
WO1998030566A1 (en) 1997-01-06 1998-07-16 Pfizer Inc. Cyclic sulfone derivatives
WO1998033768A1 (en) 1997-02-03 1998-08-06 Pfizer Products Inc. Arylsulfonylamino hydroxamic acid derivatives
WO1998034918A1 (en) 1997-02-11 1998-08-13 Pfizer Inc. Arylsulfonyl hydroxamic acid derivatives
WO1998034915A1 (en) 1997-02-07 1998-08-13 Pfizer Inc. N-hydroxy-beta-sulfonyl-propionamide derivatives and their use as inhibitors of matrix metalloproteinases
WO1999029667A1 (en) 1997-12-05 1999-06-17 Pfizer Limited Hydroxamic acid derivatives as matrix metalloprotease (mmp) inhibitors
EP0931788A2 (en) 1998-01-27 1999-07-28 Pfizer Limited Metalloprotease inhibitors
WO1999052889A1 (en) 1998-04-10 1999-10-21 Pfizer Products Inc. (4-arylsulfonylamino)-tetrahydropyran-4-carboxylic acid hydroxamides
WO1999052910A1 (en) 1998-04-10 1999-10-21 Pfizer Products Inc. Bicyclic hydroxamic acid derivatives
WO2013035754A1 (en) 2011-09-05 2013-03-14 中外製薬株式会社 Method for producing coumarin derivative
WO2023211812A1 (en) * 2022-04-25 2023-11-02 Nested Therapeutics, Inc. Heterocyclic derivatives as mitogen-activated protein kinase (mek) inhibitors
WO2025090905A1 (en) * 2023-10-26 2025-05-01 Nested Therapeutics, Inc. Crystalline forms of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one

Patent Citations (23)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US510A (en) 1837-12-07 soeel
US949A (en) 1838-09-27 Improvement in roller cotton-gins for ginning long-staple and other kinds of cotton
US5863A (en) 1848-10-17 Matthias p
US5861A (en) 1848-10-17 Locking umbrella and parasol
WO1990005719A1 (en) 1988-11-23 1990-05-31 British Bio-Technology Limited Hydroxamic acid based collagenase inhibitors
EP0606046A1 (en) 1993-01-06 1994-07-13 Ciba-Geigy Ag Arylsulfonamido-substituted hydroxamic acids
WO1996027583A1 (en) 1995-03-08 1996-09-12 Pfizer Inc. Arylsulfonylamino hydroxamic acid derivatives
WO1996033172A1 (en) 1995-04-20 1996-10-24 Pfizer Inc. Arylsulfonyl hydroxamic acid derivatives as mmp and tnf inhibitors
EP0780386A1 (en) 1995-12-20 1997-06-25 F. Hoffmann-La Roche Ag Matrix metalloprotease inhibitors
WO1998001113A1 (en) 1996-07-04 1998-01-15 Seiken Chemical Co., Ltd. Lubrication assistant and process for the preparation of ethyl stearate used therein
WO1998003516A1 (en) 1996-07-18 1998-01-29 Pfizer Inc. Phosphinate based inhibitors of matrix metalloproteases
WO1998007697A1 (en) 1996-08-23 1998-02-26 Pfizer Inc. Arylsulfonylamino hydroxamic acid derivatives
WO1998030566A1 (en) 1997-01-06 1998-07-16 Pfizer Inc. Cyclic sulfone derivatives
WO1998033768A1 (en) 1997-02-03 1998-08-06 Pfizer Products Inc. Arylsulfonylamino hydroxamic acid derivatives
WO1998034915A1 (en) 1997-02-07 1998-08-13 Pfizer Inc. N-hydroxy-beta-sulfonyl-propionamide derivatives and their use as inhibitors of matrix metalloproteinases
WO1998034918A1 (en) 1997-02-11 1998-08-13 Pfizer Inc. Arylsulfonyl hydroxamic acid derivatives
WO1999029667A1 (en) 1997-12-05 1999-06-17 Pfizer Limited Hydroxamic acid derivatives as matrix metalloprotease (mmp) inhibitors
EP0931788A2 (en) 1998-01-27 1999-07-28 Pfizer Limited Metalloprotease inhibitors
WO1999052889A1 (en) 1998-04-10 1999-10-21 Pfizer Products Inc. (4-arylsulfonylamino)-tetrahydropyran-4-carboxylic acid hydroxamides
WO1999052910A1 (en) 1998-04-10 1999-10-21 Pfizer Products Inc. Bicyclic hydroxamic acid derivatives
WO2013035754A1 (en) 2011-09-05 2013-03-14 中外製薬株式会社 Method for producing coumarin derivative
WO2023211812A1 (en) * 2022-04-25 2023-11-02 Nested Therapeutics, Inc. Heterocyclic derivatives as mitogen-activated protein kinase (mek) inhibitors
WO2025090905A1 (en) * 2023-10-26 2025-05-01 Nested Therapeutics, Inc. Crystalline forms of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
"Handbook of Pharmaceutical Excipients", 2005, PHARMACEUTICAL PRESS
"Remington's Pharmaceutical Sciences", 2003
"The United States Pharmacopeia: The National Formulary", 1999
GOODMANGILMAN: "The Pharmacological Basis of Therapeutics", MACK PUBLISHING CO.

Similar Documents

Publication Publication Date Title
KR102210316B1 (en) Bcl-2bcl-xl inhibitors and therapeutic methods using the same
JP2020516620A (en) Ferroportin inhibitor salt
US10124002B2 (en) Crystalline forms of tyrosine kinase inhibitors and their salts
TW201632504A (en) Solid forms of 2-(5-(3-fluorophenyl)-3-hydroxypicolinamido)acetic acid, compositions, and uses thereof
US20250179057A1 (en) Mek immune oncology inhibitors and therapeutic uses thereof
TW202012391A (en) Biaryl ether type quinazoline derivatives
WO2023211812A1 (en) Heterocyclic derivatives as mitogen-activated protein kinase (mek) inhibitors
KR20250174628A (en) Crystalline methionine adenosyltransferase 2a (MAT2A) inhibitors and uses thereof
EP3597186B1 (en) Myc g-quadruplex stabilizing small molecules and their use
US10301271B2 (en) Crystalline forms of tyrosine kinase inhibitors and their salts
WO2025090905A1 (en) Crystalline forms of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]methyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one
CZ2009570A3 (en) Preparation, stabilization and use of imatinib mesylate polymorphs for development of medicinal forms
EP4399207B1 (en) Crystalline forms of quinazoline derivatives, preparation, composition and use thereof
WO2025259841A1 (en) Crystalline forms of 3-[[3-fluoro-2-(methylsulfamoylamino)-4-pyridyl]jmethyl]-7-[(3-fluoro-2-pyridyl)oxy]-4-methyl-chromen-2-one
IL324168A (en) Heterocyclic derivative as a mitogen-activated protein kinase (mek) inhibitor
JP5748745B2 (en) Substituted benzotriazines and quinoxalines as inhibitors of p70S6 kinase
JP2020073523A (en) Salts and polymorphs of substituted imidazopyridinyl-aminopyridine compounds
US20250289811A1 (en) Heterocyclic derivatives as mitogen-activated protein kinase (mek) inhibitors
WO2026021545A1 (en) Salt of atr kinase inhibitor, solid form thereof, and preparation method therefor and use thereof
JP2022504201A (en) Malonic acid salt of varitinib
HK1234747B (en) Salts and polymorphs of a substituted imidazopyridinyl-aminopyridine compound

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 25743911

Country of ref document: EP

Kind code of ref document: A1