HRID2226255

反应详情

EQUATION

反应方程式

HRID 2226255 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4.45 g of 2-mercaptobenzthiazole and 5 g of but-3-ene-1,2,3-tricarboxylic acid are ground with one another in a mortar. The powdered mixture is introduced in portions and with stirring into 60 ml of 70% H2SO4 at 48°-50°, in the course of one hour. After a further 3 hours at 48°-50°, the reaction mixture is cooled to room temperature and diluted with 250 ml of water at 25°-30°, with stirring. The aqueous solution is decanted from a little tacky deposit and is diluted with a further 200 ml of water. After being stirred for 1 hour the precipitate is filtered off and dried. The 4-(benzthiazol-2-ylthio)-butane-1,2,3-tricarboxylic acid obtained melts at 188°-190° after recrystallisation from methanol/water.

WORKUP

后处理

  1. additionThe powdered mixture is introduced in portions
  2. customThe aqueous solution is decanted from a little tacky deposit
  3. additionis diluted with a further 200 ml of water
  4. stirringAfter being stirred for 1 hour the precipitate
  5. filtrationis filtered off
  6. customdried