Phosgene → HCID 54090647, 화합물

HRID 972156노트

반응식

HRID 972156 반응식
[C:1](Cl)(Cl)=[O:2].[CH:5]1([C:10]2[S:14][C:13]([NH2:15])=[N:12][N:11]=2)[CH2:9][CH2:8][CH2:7][CH2:6]1>C(OCC)(=O)C>[CH:5]1([C:10]2[S:14][C:13]([N:15]=[C:1]=[O:2])=[N:12][N:11]=2)[CH2:6][CH2:7][CH2:8][CH2:9]1

참가 물질

4

반응물 2

HCID 6371PhosgeneHCID 20636875-cyclopentyl-1,3,4-thiadiazol-2-amine

생성물 1

HCID 54090647HCID 54090647, 화합물

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매2회

실험 절차

A saturated solution of phosgene in ethyl acetate (100 ml) is charged into a glass reaction vessel equipped with a mechanical stirrer. A slurry of 5-cyclopentyl-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-cyclopentyl-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-4a6ec05f4ab5472aa0729f7fed51816e
출처 데이터셋
uspto-grants-1977_10
특허 번호
US04052191

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