HRID46629

反应详情

EQUATION

反应方程式

HRID 46629 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 1.37 g (18 mmoles) of thioacetic acid in 30 ml of ethanol is neutralized exactly, in a nitrogen atmosphere, by the dropwise addition of a 40% strength aqueous KOH solution, and 3.7 g (15 mmoles) of 2-bromo-5-chloro-1-indanone (Example 1 (a)) are added. The reaction mixture is stirred for 1 hour at room temperature and poured into 200 ml of water. The product which crystallizes after some time is filtered off and introduced, under nitrogen, into 35 ml of a 5% strength aqueous NaOH solution. After stirring for 1 hour at room temperature, the pH is adjusted to 1 with 2 N hydrochloric acid and the crystalline precipitate is filtered off. The resulting 5-chloro-2-mercapto-1-indanone decomposes at 173°-175° C.

WORKUP

后处理

  1. additionare added
  2. customThe product which crystallizes after some time
  3. filtrationis filtered off
  4. additionintroduced, under nitrogen, into 35 ml of a 5% strength aqueous NaOH solution
  5. stirringAfter stirring for 1 hour at room temperature
  6. filtrationthe crystalline precipitate is filtered off
  7. customdecomposes at 173°-175° C.