HRID353182
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
117 g of triethylamine and 140 g of 2,4-dimethylaniline are dissolved in 2 l of methylene chloride, and a solution of 233 g of alpha-bromoacetyl bromide in 400 ml of methylene chloride is added with ice-cooling, at at most 15° C., within 30 min. After a reaction time of 30 min, the precipitate is filtered off with suction, the residue is dissolved in 3 l of methylene chloride and combined with the filtrate and washed twice with 2 l of water and 2 l of sat. sodium chloride solution. The mixture is dried over sodium sulphate, filtered off with suction and concentrated, and the residue is recrystallized from ethanol. This gives 193 g of the title compound.
WORKUP
后处理
- temperaturecooling, at at most 15° C., within 30 min
- filtrationAfter a reaction time of 30 min, the precipitate is filtered off with suction
- dissolutionthe residue is dissolved in 3 l of methylene chloride
- washwashed twice with 2 l of water and 2 l of sat. sodium chloride solution
- dry with materialThe mixture is dried over sodium sulphate
- filtrationfiltered off with suction
- concentrationconcentrated
- customthe residue is recrystallized from ethanol