反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customthe aqueous phase is separated
- extractionThe aqueous phase is again extracted with 2,2-difluoro-1-chloroethane
- distillationthe combined organic phases are distilled
- additioncan be converted back into free 4-methylbenzylamine by addition of sodium hydroxide solution
- distillationAfter distillation, 4.3 g of 2,2-difluoro-N-(4-methylbenzyl)ethanamine
- customare obtained