HRID1383059
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
CONDITIONS
反应条件
- 温度
- 120 °C
PROCEDURE
实验过程
A solution of 8.63 g of 2-chloro-5-nitroaniline and 9.9 g of sodium sulphide trihydrate in 80 ml of butyl glycol was stirred at 80° C. for 30 minutes. After adding 4.16 ml of concentrated sulphuric acid, 7.6 g of thiourea were added to the 2-amino-4-nitrothiophenol, and the mixture was stirred at 120° C. for 3 hours. The reaction mixture was discharged into 400 ml of water and 50 ml of methanol, and the solid was filtered off with suction and washed with water. 5.4 g of crude 2-amino-5-nitrobenzothiazole, the identity of which was confirmed by TLC comparison with authentic material, were obtained.
WORKUP
后处理
- filtrationthe solid was filtered off with suction
- washwashed with water
- customwere obtained