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

HRID 441907
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HRID 441907 반응식
[C:1](Cl)(Cl)=[O:2].[CH2:5]([C:11]1[S:15][C:14]([NH2:16])=[N:13][N:12]=1)[CH2:6][CH2:7][CH2:8][CH2:9][CH3:10]>C(OCC)(=O)C>[CH2:5]([C:11]1[S:15][C:14]([N:16]=[C:1]=[O:2])=[N:13][N:12]=1)[CH2:6][CH2:7][CH2:8][CH2:9][CH3:10]
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참가 물질

4

반응물 2

HCID 6371PhosgeneHCID 18950395-Hexyl-1,3,4-thiadiazol-2-amine

생성물 1

HCID 539065275-Hexyl-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 glass reaction vessel equipped with a mechanical stirrer. A slurry of 5-hexyl-2-amino-1,3,4-thiadiazole (40 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-hexyl-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-a11c7c9deee94c7384e5051cb9215966
출처 데이터셋
uspto-grants-1977_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04043795

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