Phosgene → 1,3,4-Thiadiazole, 2-isocyanato-5-(trifluoromethyl)-, dimer

HRID 259125

반응식

HRID 259125 반응식
[C:1](Cl)(Cl)=[O:2].[F:5][C:6]([F:14])([F:13])[C:7]1[S:11][C:10]([NH2:12])=[N:9][N:8]=1>C(OCC)(=O)C>[C:1](=[O:2])=[N:12][C:10]1[S:11][C:7]([C:6]([F:14])([F:13])[F:5])=[N:8][N:9]=1.[C:1](=[O:2])=[N:12][C:10]1[S:11][C:7]([C:6]([F:14])([F:13])[F:5])=[N:8][N:9]=1

참가 물질

4

반응물 2

HCID 6371PhosgeneHCID 826341,3,4-Thiadiazol-2-amine, 5-(trifluoromethyl)-

생성물 1

HCID 768718351,3,4-Thiadiazole, 2-isocyanato-5-(trifluoromethyl)-, dimer

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매2회

실험 절차

A saturated solution of phosgene in ethyl acetate (100 ml) was charged into a glass reaction vessel equipped with a mechanical stirrer. A slurry of 5-trifluoromethyl-2-amino-1,3,4-thiadiazole (45 grams) in ethyl acetate (300 ml) was added to the reaction vessel, and the resulting mixture was stirred for a period of about 16 hours resulting in the formation of precipitate. The reaction mixture was then purged with nitrogen gas to remove unreacted phosgene. The purged mixture was filtered to recover 48 grams of a white solid. This solid was recrystallized from dimethyl formamide to yield the desired product 5-trifluoromethyl-1,3,4-thiadiazol-2-yl isocyanate dimer.

후처리

  1. customequipped with a mechanical stirrer
  2. customresulting in the formation of precipitate
  3. customThe reaction mixture was then purged with nitrogen gas
  4. customto remove unreacted phosgene
  5. filtrationThe purged mixture was filtered
  6. customto recover 48 grams of a white solid
  7. customThis solid was recrystallized from dimethyl formamide

출처 및 근거

ORD 기록
ord-1236806236344481b55dfe79995273e2
출처 데이터셋
uspto-grants-1977_07
특허 번호
US04036848

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