HRID1388501

反应详情

EQUATION

反应方程式

HRID 1388501 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. additionDuring this addition
  2. customis kept at 150° C.
  3. customby removing some of the distillate
  4. temperatureunder reflux for about 12 hours
  5. stirringstirred into 1.2 l of ice-water
  6. customthe 2-mercaptobenzothiazole which has precipitated
  7. filtrationis filtered off
  8. washAfter washing
  9. customdrying