HRID435604

反应详情

EQUATION

反应方程式

HRID 435604 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 855 g of potassium hydroxide in 7 litres of water are added, at 50° C under argon, 420 g of thiophenol and the mixture is stirred for 15 minutes. There are then added thereto 22.1 g of copper powder and 1 kg of 2-iodo-5--methyl-benzoic acid and the mixture is heated for 7 hours under reflux. After cooling, the mixture is adjusted to pH 3 with 600 ml of concentrated hydrochloric acid and extracted with methylene chloride, washed with water, dried over sodium sulphate and concentrated to a thick crystal mash. This is filtered under suction, washed with cold ethanol and low--boiling petroleum ether and dried. Thee is obtained 3--methyl-6-(phenylthio)-benzoic acid of melting point 156°-157° C.

WORKUP

后处理

  1. additionThere are then added
  2. temperatureunder reflux
  3. temperatureAfter cooling
  4. extractionextracted with methylene chloride
  5. washwashed with water
  6. dry with materialdried over sodium sulphate
  7. concentrationconcentrated to a thick crystal mash
  8. filtrationThis is filtered under suction
  9. washwashed with cold ethanol
  10. customdried