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SE431873B - PROCEDURE FOR PREPARING ALFA FORM OF PRAZOSINE HYDROCHLORIDE - Google Patents

PROCEDURE FOR PREPARING ALFA FORM OF PRAZOSINE HYDROCHLORIDE

Info

Publication number
SE431873B
SE431873B SE8101265A SE8101265A SE431873B SE 431873 B SE431873 B SE 431873B SE 8101265 A SE8101265 A SE 8101265A SE 8101265 A SE8101265 A SE 8101265A SE 431873 B SE431873 B SE 431873B
Authority
SE
Sweden
Prior art keywords
water
hydrochloride
procedure
hydrate
prazosin hydrochloride
Prior art date
Application number
SE8101265A
Other languages
Swedish (sv)
Other versions
SE8101265L (en
Inventor
P J Kairisalo
H Thaler
E J Honkanen
Original Assignee
Orion Yhtymae Oy
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 Orion Yhtymae Oy filed Critical Orion Yhtymae Oy
Publication of SE8101265L publication Critical patent/SE8101265L/en
Publication of SE431873B publication Critical patent/SE431873B/en

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
    • C07D405/14—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 three or more hetero rings
    • 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

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
  • Plural Heterocyclic Compounds (AREA)

Description

15 20 25 30 35 8101265-0 i 2 Oförutsett observerades att ren M-form av prazosinhydro- klorid kan framställas med kvantitativt utbyte och mycket enkelt så, att från prazosinhydrokloridens hydrat eller vat- tenhaltiga hydrat vattnet avlägsnas genom azeotropisk des- tillation tillsammans med diklormetan och det frigjorda vatt- net separeras under användning av en vattenavskiljare. Här- vid konstaterades det att enbart a-formen av prazosinhydro- klorid bildades. Produkten identifierades på basen av dess IR-spektrum. Unexpectedly, it was observed that pure M-form of prazosin hydrochloride can be prepared in quantitative yield and very simply so that from the hydrate or aqueous hydrate of the prazosin hydrochloride the water is removed by azeotropic distillation together with dichloromethane. and the liberated water is separated using a water separator. It was found that only the α-form of prazosin hydrochloride was formed. The product was identified on the basis of its IR spectrum.

Det uppfinningsenliga förfarandet är fördelaktigt fram- för allt på grund av den laga temperaturen (ca 420). En extra fördel är att diklormetanet är ett billigt, lätt regene- rerbart och för industriellt bruk synnerligen lämpligt lös- ningsmedel. Bildning av föroreningar har icke observerats vid det uppfinningsenliga förfarandet.The process according to the invention is advantageous above all due to the low temperature (approx. 420). An additional advantage is that the dichloromethane is a cheap, easily regenerable and extremely suitable solvent for industrial use. The formation of impurities has not been observed in the process according to the invention.

Följande exempel illustrerar uppfinningen.The following examples illustrate the invention.

Exempel 1. 228 g (0,5 mol) dihydrat av prazosinhydroklorid(framställt med det i svenska patentet 423 234 anförda förfarandet) uppslammas i 2200 ml diklormetan. Till reaktionskärlet an- slutes en vattenavskiljare och blandningen kokas under äter- lopp tills vatten icke längre avskiljs (ca 4...6 h). Fäll- .ningen avfiltreras och det kvarblivande diklormetanet avduns- tas under nedsatt tryck. Erhàlles 210 g_(100 % av det teore- tiska) prazosinhydroklorid (sönd.p. 280...82°, IR (KBr): 3319, 3226, 3077, 2857, 1634, 1597,-1481, 1468, 1425, 1280, 794, 763, 751, 721, 717, 675 cm_1). IR-spektret är identiskt med den i patentansökningen FI 77 0634 beskrivna u-formens spektrum.Example 1. 228 g (0.5 mol) of dihydrate of prazosin hydrochloride (prepared by the process cited in Swedish patent 423 234) are slurried in 2200 ml of dichloromethane. A water separator is connected to the reaction vessel and the mixture is boiled under reflux until water is no longer separated (approx. 4 ... 6 h). The precipitate is filtered off and the remaining dichloromethane is evaporated off under reduced pressure. Obtained 210 g (100% of theory) of prazosin hydrochloride (Sun.p. 280 ... 82 °, IR (KBr): 3319, 3226, 3077, 2857, 1634, 1597, -1481, 1468, 1425, 1280 , 794, 763, 751, 721, 717, 675 cm_1). The IR spectrum is identical to the spectrum of the u-shape described in patent application FI 77 0634.

Exempel 2. 300 g otorkad från vattenhaltigt medium filtrerad och med vatten tvättad prazosinhydroklorid (inneh. 30 % vatten enligt Karl Fischers bestämningsmetod) uppslammas i 2200 ml diklormetan och förfares på samma sätt som i exemplet 1. Er- hálles 210 g (100 % av det teoretiska) a-pratzosinhydroklo- rid.Example 2. 300 g of undried aqueous medium filtered and water-washed prazosin hydrochloride (containing 30% of water according to Karl Fischers method of determination) are suspended in 2200 ml of dichloromethane and proceed in the same manner as in Example 1. 210 g (100% of the theoretical) α-pratzosin hydrochloride.

Claims (2)

8101265-0 Patentkrav8101265-0 Patent claims 1. Förfarande för framställning av a-form av 2-ÄÉ-(2-furoyl) piperazin-1-yl]-4-amino-6,7-dimetoxikinazolin-hydroklorid, k ä n n e- t e c k n a d därav, att kristallvattnet i prazosinhydrokloridens hydrat avlägsnas azeotropiskt, genom att koka hydratet i diklormetan och separera det frigjorda vattnet under användning av vattenavskil- jare.A process for the preparation of α-form of 2- [2- (2-furoyl) piperazin-1-yl] -4-amino-6,7-dimethoxyquinazoline hydrochloride, characterized in that the crystalline water of prazosin hydrochloride hydrate is removed azeotropically, by boiling the hydrate in dichloromethane and separating the liberated water using water separators. 2. Förfarande enligt patentkravet 1, k ä n n e t e c k n a t därav, att som utgångsämne användes dihydrat av prazosinhydroklorid. Sammandrag En process för framstäïlnïng av CK-formen av prazosinhydroklorïd, NW ___co____í 9\fi N '- _2 beskrivs. Krïstaïlvattnet i ett hydrat av prazosínhydrokloríd avïägsnas azeotropískt, genom att koka hydratet ï díklormetan och separera de fri- gjorda vattnet under användning av en vattenavskïljare.Process according to Claim 1, characterized in that dihydrate of prazosin hydrochloride is used as starting material. Abstract A process for the preparation of the CK form of prazosin hydrochloride, NW ___ co ____ í 9 \ fi N '- _2 is described. The crystalline water in a hydrate of prazosin hydrochloride is azeotropically removed by boiling the hydrate in dichloromethane and separating the liberated water using a water separator.
SE8101265A 1980-02-26 1981-02-26 PROCEDURE FOR PREPARING ALFA FORM OF PRAZOSINE HYDROCHLORIDE SE431873B (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
FI800556A FI64367C (en) 1980-02-26 1980-02-26 OIL FRAMSTAELLNING AV ALFA FORM AV PRAZOSINHYDROCHLORIDE

Publications (2)

Publication Number Publication Date
SE8101265L SE8101265L (en) 1981-08-27
SE431873B true SE431873B (en) 1984-03-05

Family

ID=8513276

Family Applications (1)

Application Number Title Priority Date Filing Date
SE8101265A SE431873B (en) 1980-02-26 1981-02-26 PROCEDURE FOR PREPARING ALFA FORM OF PRAZOSINE HYDROCHLORIDE

Country Status (11)

Country Link
CS (1) CS216226B2 (en)
DD (1) DD156532A5 (en)
DK (1) DK157548C (en)
ES (1) ES499796A0 (en)
FI (1) FI64367C (en)
HU (1) HU182297B (en)
NO (1) NO154461C (en)
PL (1) PL128350B1 (en)
PT (1) PT72511B (en)
SE (1) SE431873B (en)
SU (1) SU980621A3 (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FI79107C (en) * 1984-06-25 1989-11-10 Orion Yhtymae Oy Process for the preparation of stable form of prazosin hydrochloride.

Also Published As

Publication number Publication date
DK84581A (en) 1981-08-27
PL229865A1 (en) 1981-10-30
DK157548C (en) 1990-06-11
PL128350B1 (en) 1984-01-31
FI64367B (en) 1983-07-29
FI800556A (en) 1981-08-27
DD156532A5 (en) 1982-09-01
HU182297B (en) 1983-12-28
ES8201577A1 (en) 1981-12-16
CS216226B2 (en) 1982-10-29
PT72511A (en) 1981-03-01
SE8101265L (en) 1981-08-27
DK157548B (en) 1990-01-22
ES499796A0 (en) 1981-12-16
NO154461C (en) 1986-09-24
SU980621A3 (en) 1982-12-07
PT72511B (en) 1983-02-01
NO154461B (en) 1986-06-16
FI64367C (en) 1986-08-05
NO810590L (en) 1981-08-27

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