HRID1854807

反应详情

EQUATION

反应方程式

HRID 1854807 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

3.29 g (30.8 mmoles) of methylamino-acetonitrile hydrochloride is placed in the presence of 19.6 g (154 mmoles) of oxalyl chloride in 30 ml of 1,2-dichlorobenzene. The mixture is heated for 8 hours at 80° C. After concentrating the reaction medium to dryness, the residue obtained is purified by flash chromatography (Petroleum ether-CH2Cl2 gradient 100-0 to 0-100). 3.35 g of intermediate 4c is obtained in beige powder form (yield: 60%).

WORKUP

后处理

  1. concentrationAfter concentrating the reaction medium to dryness
  2. customthe residue obtained
  3. customis purified by flash chromatography (Petroleum ether-CH2Cl2 gradient 100-0 to 0-100)