HRID345798

反应详情

EQUATION

反应方程式

HRID 345798 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

74.8 g (0.4 mol) of N-benzylmaleimide [Arch. Pharm. 308, 489 (1975)] and 52.0 g (0.4 mol) of 2-chloroethyl-methylamine hydrochloride are initially introduced into 400 ml of dioxane and 40.4 g (0.4 mol) of triethylamine are added dropwise at 20° C. The mixture is then boiled under reflux for 5 hours. The batch is subsequently poured into 2 l of ice-water and extracted with 3 portions of 400 ml of chloroform and the extract is washed with water, dried over sodium sulphate and concentrated on a rotary evaporator. Chromatography of the residue (101.1 g) on silica gel using ethyl acetate:petroleum ether (1:2) gives 56.8 g (51% of theory) of an oil.

WORKUP

后处理

  1. additionare added dropwise at 20° C
  2. temperatureunder reflux for 5 hours
  3. extractionextracted with 3 portions of 400 ml of chloroform
  4. washthe extract is washed with water
  5. dry with materialdried over sodium sulphate
  6. concentrationconcentrated on a rotary evaporator
  7. customgives 56.8 g (51% of theory) of an oil