HRID260502

反应详情

EQUATION

反应方程式

HRID 260502 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2(a) 2.8 ml of triethylamine were added to a suspension of 2.11 g of diethyl 2-aminomalonate hydrochloride in 50 ml of methylene chloride. 1.71 g of 3-bromopropionyl chloride were then added to the mixture, whilst ice-cooling, and then the mixture was stirred for 30 minutes. At the end of this time, the reaction mixture was poured into water and extracted with diethyl ether. The extract was washed with a 5% w/v aqueous solution of sodium bicarbonate and with water, in that order, after which it was dried over anhydrous magnesium sulfate. The solvent was then removed by distillation under reduced pressure, to give 2.5 g of diethyl 2-(3-bromopropionamido)malonate.

WORKUP

后处理

  1. temperaturecooling
  2. extractionextracted with diethyl ether
  3. washThe extract was washed with a 5% w/v aqueous solution of sodium bicarbonate and with water, in that order
  4. dry with materialafter which it was dried over anhydrous magnesium sulfate
  5. customThe solvent was then removed by distillation under reduced pressure