HRID2418496

反应详情

EQUATION

反应方程式

HRID 2418496 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 25 g o-mercaptobenzyl alcohol (0.18 mole), 39.6 g 3-iodo-4-hydroxy benzoic acid (0.15 mole), 11.43 g copper powder (0.18 mole), 70 ml 40% aqueous potassium hydroxide solution (0.5 mole) and 300 ml water was placed under nitrogen atmosphere and stirred under reflux for 18 hours. After cooling the mixture was diluted with 400 ml of water and extracted twice with 100 ml of ethyl acetate to remove neutral products. The aqueous fraction was filtered and the filtrate acidified with conc. HCl to afford the title compound as an oil which solidified and was filtered. There was obtained 32.8 g solid.

WORKUP

后处理

  1. temperatureunder reflux for 18 hours
  2. temperatureAfter cooling the mixture
  3. extractionextracted twice with 100 ml of ethyl acetate
  4. customto remove neutral products
  5. filtrationThe aqueous fraction was filtered