HRID37415

反应详情

EQUATION

反应方程式

HRID 37415 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

3.74 g of sodium were dissolved in 77 ml of absolute ethanol under argon. The solution was treated dropwise with 25 g of m-bromothiophenol and heated to reflux. Thereafter, 12.4 ml of γ-butyrolactone were added and the reaction mixture was heated to 110° C. for 5 hours. The separated carboxylic acid sodium salt was removed by filtration, washed with a small amount of ether and dissolved in 300 ml of water. The solution was acidified to pH 2 with 1N HCl while cooling with ice, the free carboxylic acid was extracted with ether, the ethereal solution was dried and evaporated. There were obtained 33.1 g of 4-(m-bromophenylmercapto)butyric acid.

WORKUP

后处理

  1. temperatureheated to reflux
  2. customThe separated carboxylic acid sodium salt was removed by filtration
  3. washwashed with a small amount of ether
  4. dissolutiondissolved in 300 ml of water
  5. temperaturewhile cooling with ice
  6. extractionthe free carboxylic acid was extracted with ether
  7. customthe ethereal solution was dried
  8. customevaporated