HRID1266516

反应详情

EQUATION

反应方程式

HRID 1266516 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

117 g of triethylamine and 140 g of 2,4-dimethylaniline are dissolved in 21 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

  1. temperaturecooling, at at most 15° C., within 30 min
  2. filtrationAfter a reaction time of 30 min, the precipitate is filtered off with suction
  3. dissolutionthe residue is dissolved in 3 l of methylene chloride
  4. washwashed twice with 2 l of water and 2 l of sat. sodium chloride solution
  5. dry with materialThe mixture is dried over sodium sulphate
  6. filtrationfiltered off with suction
  7. concentrationconcentrated
  8. customthe residue is recrystallized from ethanol