HRID1388531

反应详情

EQUATION

反应方程式

HRID 1388531 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

solution of 3.4 g sodium hydroxide in 6 ml of water and then 14 g of 2,5-dichlorobenzaldehyde (H. Erdmann, Justus Liebigs Ann. Chem. 272, 155, 1893) are added to a solution of 10.8 g 2-fluorothiophenol (reference above) in 20 ml of hexamethylphosphortriamide. Then, the mixture is heated for 5.5 hours to 100° C. After cooling it is diluted with 150 ml of water and extracted with benzene. The extract is washed with a 5% sodium hydroxide solution and with water, dried with magnesium sulfate and evaporated. Crude 2-(2-fluorophenylthio) 5-chlorobenzaldehyde is obtained which is then recrystallized from 20 ml ethanol; 16.0 g, m.p. 85.5°-88° C. A further crystallization affords an analytically pure product, m.p. 87°-88° C.

WORKUP

后处理

  1. temperatureThen, the mixture is heated for 5.5 hours to 100° C
  2. temperatureAfter cooling it
  3. extractionextracted with benzene
  4. washThe extract is washed with a 5% sodium hydroxide solution and with water
  5. dry with materialdried with magnesium sulfate
  6. customevaporated