HRID2098415

反应详情

EQUATION

反应方程式

HRID 2098415 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

An amount of 26.2 g (242 mmol) of 2,2-difluoro-1-chloroethane and 10 g of 4-methylbenzylamine (80.8 mmol) are heated in an autoclave at an internal temperature of 120° C. for 16 hours. Subsequently, 50 g of water are added and the aqueous phase is separated. The aqueous phase is again extracted with 2,2-difluoro-1-chloroethane and the combined organic phases are distilled as described in Example 1.1. Here also, the 4-methylbenzylamine hydrochloride which is present in the aqueous phase can be converted back into free 4-methylbenzylamine by addition of sodium hydroxide solution. After distillation, 4.3 g of 2,2-difluoro-N-(4-methylbenzyl)ethanamine are obtained, which corresponds to a yield of 58%, based on reacted 4-methylbenzylamine.

WORKUP

后处理

  1. customthe aqueous phase is separated
  2. extractionThe aqueous phase is again extracted with 2,2-difluoro-1-chloroethane
  3. distillationthe combined organic phases are distilled
  4. additioncan be converted back into free 4-methylbenzylamine by addition of sodium hydroxide solution
  5. distillationAfter distillation, 4.3 g of 2,2-difluoro-N-(4-methylbenzyl)ethanamine
  6. customare obtained