HRID1086327

反应详情

EQUATION

反应方程式

HRID 1086327 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 60 g (0.103 mol) of 2,2-bis-(4-mesyloxy-3-nitrophenyl)-hexafluoropropane and 122.8 g (1.32 mol) of aniline in 400 ml of acetonitrile is heated under reflux for 24 hours. In the course of this the methanesulfonic acid salt of aniline is precipitated, and is removed by filtration with suction. The filtrate is freed from the solvent and from excess aniline by distillation under reduced pressure. Recrystallizing the residue from ethanol gives 47.3 g of 2,2-bis-(4-anilino-3-nitrophenyl)-hexafluoropropane (80% yield). M.p. 165-166° C.

WORKUP

后处理

  1. temperatureunder reflux for 24 hours
  2. customIn the course of this the methanesulfonic acid salt of aniline is precipitated
  3. customis removed by filtration with suction
  4. distillationThe filtrate is freed from the solvent and from excess aniline by distillation under reduced pressure
  5. customRecrystallizing the residue from ethanol