NO127137B - - Google Patents
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- Publication number
- NO127137B NO127137B NO36369A NO36369A NO127137B NO 127137 B NO127137 B NO 127137B NO 36369 A NO36369 A NO 36369A NO 36369 A NO36369 A NO 36369A NO 127137 B NO127137 B NO 127137B
- Authority
- NO
- Norway
- Prior art keywords
- methylthiophenthiazine
- methylthiodiphenylamine
- melting point
- cooled
- mixture
- Prior art date
Links
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 2
- 238000007363 ring formation reaction Methods 0.000 claims description 2
- 239000005864 Sulphur Substances 0.000 claims 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 238000002844 melting Methods 0.000 description 5
- 230000008018 melting Effects 0.000 description 5
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- WJFKNYWRSNBZNX-UHFFFAOYSA-N 10H-phenothiazine Chemical class C1=CC=C2NC3=CC=CC=C3SC2=C1 WJFKNYWRSNBZNX-UHFFFAOYSA-N 0.000 description 1
- 241001480043 Arthrodermataceae Species 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000006114 decarboxylation reaction Methods 0.000 description 1
- 230000037304 dermatophytes Effects 0.000 description 1
- 230000000855 fungicidal effect Effects 0.000 description 1
- 239000000417 fungicide Substances 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
Classifications
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B21/00—Arrangements or duct systems, e.g. in combination with pallet boxes, for supplying and controlling air or gases for drying solid materials or objects
- F26B21/06—Controlling, e.g. regulating, parameters of gas supply
- F26B21/08—Humidity
- F26B21/083—Humidity by using sorbent or hygroscopic materials, e.g. chemical substances, molecular sieves
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/48—Sulfur dioxide; Sulfurous acid
- C01B17/50—Preparation of sulfur dioxide
- C01B17/56—Separation; Purification
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/69—Sulfur trioxide; Sulfuric acid
- C01B17/74—Preparation
- C01B17/76—Preparation by contact processes
- C01B17/80—Apparatus
- C01B17/806—Absorbers; Heat exchangers
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Gas Separation By Absorption (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
- Drying Of Gases (AREA)
- Treating Waste Gases (AREA)
Description
Fremgangsmåte for fremstilling av 3-metyltiofentiazin. Process for the production of 3-methylthiophenthiazine.
Nærværende oppfinnelse angår en The present invention relates to a
fremgangsmåte for fremstilling av fentia-zinderivatet 3-metyltiofentiazin. method for producing the phenthiazine derivative 3-methylthiophenthiazine.
Ifølge oppfinnelsen fremstilles 3-metyltiofentiazin (Beilstein-nomenklatur), en According to the invention, 3-methylthiophenthiazine (Beilstein nomenclature) is produced, a
hittil ukjent forbindelse ved syklisering av hitherto unknown compound by cyclization of
3-metyltiodifenylamin med svovel. 3-methylthiodiphenylamine with sulfur.
3-metyltiofentiazin er et viktig indu-strielt kjemikalium. Det kan brukes som 3-Methylthiophenthiazine is an important industrial chemical. It can be used as
vulkaniseringsaksellerator, antioksydant vulcanization accelerator, antioxidant
for smøremidler, som anthelmintica og som for lubricants, as anthelmintica and as
fungicid, særlig mot dermatofyter. Det er fungicide, especially against dermatophytes. It is
også verdifullt som mellomprodukt for also valuable as an intermediate for
fremstilling av terapeutisk anvendelige N-aminoalkylfentiaziner. preparation of therapeutically useful N-aminoalkylphenthiazines.
Oppfinnelsen illustreres ved det føl-gende utførelseseksempel, i hvilket smelte-punktene som er angitt, er bestemt med The invention is illustrated by the following embodiment example, in which the melting points indicated are determined with
Koflerapparat. Kofler apparatus.
Eksempel: 3-metyltiodifenylamin (539 g) blan-des intimt med svovel (160,4 g) og etter til-setting av noen få milligram jod, oppvar-mes blandingen til 175° C i 4 timer i nitro-genatmosfære og økes deretter gradvis i Example: 3-methylthiodiphenylamine (539 g) is intimately mixed with sulfur (160.4 g) and after the addition of a few milligrams of iodine, the mixture is heated to 175° C. for 4 hours in a nitrogen atmosphere and then increased gradually i
løpet av 45 minutter til 225° C. Utvikling during 45 minutes at 225° C. Development
av svovelvannstoff har hørt opp når denne of hydrogen sulphide has stopped when this
temperatur er nådd, og blandingen kjøles temperature is reached, and the mixture is cooled
til 150° C og helles i kokende metanol (2500 cm<*>). En uoppløselig olje skiller seg ut, oppløsningen kjøles til ca. 15° C og får henstå i 17 timer ved denne temperatur. Etter at den metanoliske oppløsning er de-kantert, konsentreres den under redusert trykk. Ca. 2200 cm<:1> metanol destilleres av, og innholdet av flasken kjøles derpå til 10° C og filtreres. Der oppnås slik gule krystal-ler (509 g), smeltepunkt 126° C. to 150° C and poured into boiling methanol (2500 cm<*>). An insoluble oil separates, the solution is cooled to approx. 15° C and allowed to stand for 17 hours at this temperature. After the methanolic solution is decanted, it is concentrated under reduced pressure. About. 2200 cm<:1> methanol is distilled off, and the contents of the bottle are then cooled to 10° C and filtered. Yellow crystals (509 g), melting point 126° C, are thus obtained.
Rensning kan utføres ved omkrystalli-sering fra etanol og fra en blanding av ben-zol og heptan. 3-metyltiofentiazin (230 g) oppnås tilslutt, smeltepunkt 136° C. Purification can be carried out by recrystallization from ethanol and from a mixture of benzene and heptane. 3-Methylthiophenthiazine (230 g) is finally obtained, melting point 136° C.
Utgangs 3-metyltiodifenylaminet (ko-kepunkt 160—186° C/0,12 mm Hg og smeltepunkt 58° C) oppnås ved dekarboksyle-ring av 2-karboksy-3'-metyltiodifenylamin, smeltepunkt 140—141° C. The starting 3-methylthiodiphenylamine (boiling point 160-186° C/0.12 mm Hg and melting point 58° C) is obtained by decarboxylation of 2-carboxy-3'-methylthiodiphenylamine, melting point 140-141° C.
Claims (1)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE1968M0077146 DE1719559B2 (en) | 1968-02-03 | 1968-02-03 | ABSORPTION DEVICE |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| NO127137B true NO127137B (en) | 1973-05-14 |
Family
ID=7317458
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| NO36369A NO127137B (en) | 1968-02-03 | 1969-01-30 |
Country Status (8)
| Country | Link |
|---|---|
| BE (1) | BE727810A (en) |
| CA (1) | CA926771A (en) |
| DE (1) | DE1719559B2 (en) |
| ES (1) | ES362642A1 (en) |
| NL (1) | NL6901613A (en) |
| NO (1) | NO127137B (en) |
| SE (1) | SE361826B (en) |
| YU (1) | YU32910B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2740039A1 (en) * | 1977-09-06 | 1979-03-15 | Heinz Hoelter | Two=stage gas scrubber - with acid and alkaline treatment branch over common fluid sump |
| FR2457456A1 (en) * | 1979-05-23 | 1980-12-19 | Commissariat Energie Atomique | Drying prods, esp. agricultural prods. - by circulating through prod. air dried and heated by contact with water-absorbent soln. conc. by solar energy |
| FI62002C (en) * | 1981-04-15 | 1982-11-10 | Outokumpu Oy | REFERENCE FITTING FOR SEPARATION OF A QUANTIFIED HYDROGEN WITH HYDROGEN GASER |
| FR2938448B1 (en) * | 2008-11-20 | 2014-09-26 | Total Raffinage Marketing | DEVICE AND METHOD FOR GAS TREATMENT AND COMPRESSION |
| DE102008058637B4 (en) | 2008-11-22 | 2017-01-05 | Outotec Oyj | separating |
-
1968
- 1968-02-03 DE DE1968M0077146 patent/DE1719559B2/en active Granted
- 1968-12-27 SE SE1788968A patent/SE361826B/xx unknown
-
1969
- 1969-01-17 ES ES362642A patent/ES362642A1/en not_active Expired
- 1969-01-30 NO NO36369A patent/NO127137B/no unknown
- 1969-01-30 CA CA041615A patent/CA926771A/en not_active Expired
- 1969-01-31 NL NL6901613A patent/NL6901613A/xx unknown
- 1969-01-31 BE BE727810D patent/BE727810A/xx unknown
- 1969-02-03 YU YU24669A patent/YU32910B/en unknown
Also Published As
| Publication number | Publication date |
|---|---|
| CA926771A (en) | 1973-05-22 |
| DE1719559B2 (en) | 1976-12-02 |
| BE727810A (en) | 1969-07-01 |
| NL6901613A (en) | 1969-08-05 |
| SE361826B (en) | 1973-11-19 |
| DE1719559A1 (en) | 1972-02-24 |
| YU24669A (en) | 1975-04-30 |
| ES362642A1 (en) | 1970-11-16 |
| YU32910B (en) | 1975-10-31 |
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