Hydrochloric Acid → 4-Chlorothiobenzamide
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]=1참가 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
- temperaturewhile being chilled in an ice bath
- distillationThe mixture was then distilled slowly on an oil bath at 100° C
- customWhen the liquid had been removed
- additionaqueous sodium bicarbonate was added
- customThe solid was collected
- customrecrystallized from toluene
출처 및 근거
- ORD 기록
- ord-779b64027b4342e8b5465d74100591ca
- 출처 데이터셋
- uspto-grants-1985_10
- 특허 번호
- US04544759
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