HRID465286

反应详情

EQUATION

反应方程式

HRID 465286 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

20.9 g of 2-methyleneglutaric acid are dissolved at 50°, with stirring, in 150 ml of 75% H2SO4, and 24.2 g of 2-mercaptobenzthiazole are added slowly. The reaction is exothermic and the temperature rises to 60°. The reaction mixture is then stirred for 2 hours at 55°. The resulting brown solution is poured into 500 ml of water and stirred for 1 hour. 600 ml of water are then added, and the white precipitate is filtered off. Recrystallisation from aqueous methanol gives 4-(benzthiazol-2-ylthio)-butane-1,3-dicarboxylic acid, melting at 152°-154°.

WORKUP

后处理

  1. customrises to 60°
  2. stirringstirred for 1 hour
  3. filtrationthe white precipitate is filtered off
  4. customRecrystallisation from aqueous methanol