HRID977909

反应详情

EQUATION

反应方程式

HRID 977909 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 gm o-mercaptobenzyl alcohol (0.18 mole), 39.6 gm 3-iodo-4-hydroxy benzoic acid (0.15 mole), 11.43 g copper powder (0.18 mole), 70 cc 40% aqueous potassium hydroxide solution (0.5 mole) and 300 cc water was placed under nitrogen atmosphere and stirred under reflux for 18 hours. After cooling the mixture was diluted with 400 cc of water and extracted twice with 100 cc 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 of solid product.

WORKUP

后处理

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