Hydrochloric Acid → 4-Chlorothiobenzamide

HRID 463882노트

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HRID 463882 반응식
[Cl:1][C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[CH:4][CH:3]=1.C(N)(=[S:12])C.Cl>CN(C)C=O>[Cl:1][C:2]1[CH:9]=[CH:8][C:5]([C:6]([NH2:7])=[S:12])=[CH:4][CH:3]=1

참가 물질

5

실험 절차

A mixture of 55.03 g of 4-chlorobenzonitrile, 75.13 g of thioacetamide and 600 ml of dimethylformamide was saturated with dry hydrogen chloride gas while being chilled in an ice bath. The mixture was then distilled slowly on an oil bath at 100° C. When the liquid had been removed, aqueous sodium bicarbonate was added. The solid was collected and recrystallized from toluene, giving 48.35 g of 4-chlorothiobenzamide as yellow crystals.

후처리

  1. temperaturewhile being chilled in an ice bath
  2. distillationThe mixture was then distilled slowly on an oil bath at 100° C
  3. customWhen the liquid had been removed
  4. additionaqueous sodium bicarbonate was added
  5. customThe solid was collected
  6. customrecrystallized from toluene

출처 및 근거

ORD 기록
ord-779b64027b4342e8b5465d74100591ca
출처 데이터셋
uspto-grants-1985_10
특허 번호
US04544759

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