HRID637811

反应详情

EQUATION

反应方程式

HRID 637811 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A 194 g (1.1 moles) quantity of 4-fluorobenzenesulfonic acid was added to 96 g (1 mole) of fluorobenzene and the mixture was cooled with water while 123 g (1.1 moles) of chlorosulfonic acid was added at about 10° to about 20° C. over a period of 1 hour. After the addition, the reaction mixture was stirred for 3 hours while being maintained at 20° to 30° C. The hydrochloric acid gas evolved during the reaction was continuously removed from the reaction system. After the completion of the reaction, about 400 ml of water was added to the reaction mixture, and 9.6 g (0.1 mole) of the unreacted fluorobenzene was recovered by distillation. Separation of the precipitate by filtration gave 65 g of 4,4'-difluorodiphenylsulfone in 58% yield. M.P. 97° to 98° C. Purity of 99.7%.

WORKUP

后处理

  1. additionwas added at about 10° to about 20° C. over a period of 1 hour
  2. additionAfter the addition
  3. temperaturewhile being maintained at 20° to 30° C
  4. customwas continuously removed from the reaction system
  5. customAfter the completion of the reaction, about 400 ml of water
  6. distillationwas recovered by distillation
  7. customSeparation of the precipitate
  8. filtrationby filtration