HRID463882
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
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.
WORKUP
后处理
- 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