Phosgene → 5-Cycloheptyl-1,3,4-thiadiazol-2-yl isocyanate

HRID 596738노트

반응식

HRID 596738 반응식
[C:1](Cl)(Cl)=[O:2].[CH:5]1([C:12]2[S:16][C:15]([NH2:17])=[N:14][N:13]=2)[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6]1>C(OCC)(=O)C>[CH:5]1([C:12]2[S:16][C:15]([N:17]=[C:1]=[O:2])=[N:14][N:13]=2)[CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11]1

참가 물질

4

반응물 2

HCID 6371PhosgeneHCID 214478325-Cycloheptyl-2-amino-1,3,4-thiadiazole

생성물 1

HCID 214819185-Cycloheptyl-1,3,4-thiadiazol-2-yl isocyanate

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매2회

실험 절차

A saturated solution of phosgene in ethyl acetate (100 ml) is charged into a class reaction vessel equipped with a mechanical stirrer. A slurry of 5-cycloheptyl-2-amino-1,3,4-thiadiazole (50 grams) in ethyl acetate (300 ml) is added to the reaction vessel and the resulting mixture is stirred for a period of about 16 hours, resulting in the formation of a precipitate. The reaction mixture is then purged with nitrogen gas to remove unreacted phosgene. The purged mixture is then filtered to recover the precipitate. The precipitate is then recrystallized to yield the desired product 5-cycloheptyl-1,3,4-thiadiazol-2-yl isocyanate dimer.

후처리

  1. customequipped with a mechanical stirrer
  2. customresulting in the formation of a precipitate
  3. customThe reaction mixture is then purged with nitrogen gas
  4. customto remove unreacted phosgene
  5. filtrationThe purged mixture is then filtered
  6. customto recover the precipitate
  7. customThe precipitate is then recrystallized

출처 및 근거

ORD 기록
ord-9f58ca8b0e654924b6a056ed727eaf31
출처 데이터셋
uspto-grants-1977_03
특허 번호
US04012223

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