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
- 80 °C
PROCEDURE
实验过程
A solution of 216.2 g of sodium ethylxanthate in 250 ml of dimethylformamide is added dropwise to a solution, heated to 140°-150° C., of 63.8 g of 2-chloroaniline in 150 ml of dimethylformamide in the course of one hour, under a nitrogen atmosphere. During this addition, the internal temperature is kept at 150° C. by removing some of the distillate. The reaction mixture is then subsequently stirred under reflux for about 12 hours, cooled to about 80° C. and stirred into 1.2 l of ice-water. The resulting cloudy solution is acidified and the 2-mercaptobenzothiazole which has precipitated is filtered off. After washing and drying, 79 g (94.6% of theory) of 2-mercaptobenzothiazole of melting point 179°-180° C. are obtained.
WORKUP
后处理
- additionDuring this addition
- customis kept at 150° C.
- customby removing some of the distillate
- temperatureunder reflux for about 12 hours
- stirringstirred into 1.2 l of ice-water
- customthe 2-mercaptobenzothiazole which has precipitated
- filtrationis filtered off
- washAfter washing
- customdrying