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
272.1 g (976 mmol) of triphenylchloromethane, 800 ml of dichloromethane and 200 g (976 mmol) of 2-bromoethanamine hydrobromide are introduced into a 2-1 round bottom flask placed under nitrogen. The mixture is stirred and 300 ml of triethylamine are added dropwise and stirring is continued for 48 h. The triethylamine hydrochloride which precipitates is separated off, water is added to the filtrate, the organic phase is separated off and is washed with water and dried over sodium sulphate, and the solvent is evaporated off. An oil is obtained, which is purified by chromatography on a column of silica gel. After recrystallisation from a mixture of dichloromethane and cyclohexane 273.17 g of white solid are obtained. Melting point: 108°-109° C.
WORKUP
后处理
- stirringstirring
- customThe triethylamine hydrochloride which precipitates
- customis separated off
- additionwater is added to the filtrate
- customthe organic phase is separated off
- washis washed with water
- dry with materialdried over sodium sulphate
- customthe solvent is evaporated off
- customAn oil is obtained
- customwhich is purified by chromatography on a column of silica gel
- customAfter recrystallisation
- additionfrom a mixture of dichloromethane and cyclohexane 273.17 g of white solid
- customare obtained