HRID1388502

反应详情

EQUATION

反应方程式

HRID 1388502 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

91 g of carbon disulfide are added dropwise to a stirred suspension of 162 g of 2,4-dichloroaniline and 414 g of potassium carbonate in 1,000 ml of dimethylformamide at about 25°-30° C. in the course of 40 minutes, under a nitrogen atmosphere. The mixture is then warmed to an internal temperature of 150° C. in the course of 2 hours, and this temperature is maintained for 16 hours. The batch is cooled and filtered and the filtrate is largely freed from dimethylformamide. 600 ml of water are added to the residue which remains, the mixture is acidified and the product which precipitates is filtered off and dried. 187.6 g (93.2% of theory) of 6-chloro-2-mercaptobenzothiazole of melting point 258° C. are obtained.

WORKUP

后处理

  1. temperaturethis temperature is maintained for 16 hours
  2. temperatureThe batch is cooled
  3. filtrationfiltered
  4. addition600 ml of water are added to the residue which
  5. customthe product which precipitates
  6. filtrationis filtered off
  7. customdried