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Phosgene → HCID 53797236, 화합물

HRID 596742
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HRID 596742 반응식
[C:1](Cl)(Cl)=[O:2].[Cl:5][CH:6]1[CH2:11][CH2:10][CH:9]([C:12]2[S:16][C:15]([NH2:17])=[N:14][N:13]=2)[CH2:8][CH2:7]1>C(OCC)(=O)C>[Cl:5][CH:6]1[CH2:7][CH2:8][CH:9]([C:12]2[S:16][C:15]([N:17]=[C:1]=[O:2])=[N:14][N:13]=2)[CH2:10][CH2:11]1
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참가 물질

4

반응물 2

HCID 6371PhosgeneHCID 214478445-(4-Chlorocyclohexyl)-1,3,4-thiadiazol-2-amine

생성물 1

HCID 53797236HCID 53797236, 화합물

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

A saturated solution of phosgene in ethyl acetate (500 ml) is charged into a glass reaction vessel equipped with a mechanical stirrer. 5-(4-Chlorocyclohexyl)-2-amino-1,3,4-thiadiazole (6 grams) is added to the reaction vessel and the resulting mixture is stirred and heated at reflux for a period of about 4 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-(4-chlorocyclohexyl)-1,3,4-thiadiazol-2-yl isocyanate dimer.

후처리

  1. customequipped with a mechanical stirrer
  2. temperatureheated
  3. temperatureat reflux for a period of about 4 hours
  4. customresulting in the formation of a precipitate
  5. customThe reaction mixture is then purged with nitrogen gas
  6. customto remove unreacted phosgene
  7. filtrationThe purged mixture is then filtered
  8. customto recover the precipitate
  9. customThe precipitate is then recrystallized

출처 및 근거

ORD 기록
ord-079af2be69de4234b7779778648f8865
출처 데이터셋
uspto-grants-1977_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04012223

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