HRID914953

反应详情

EQUATION

反应方程式

HRID 914953 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

A mixture of 3-hydroxy picolinic amide (10 g, 72 mmol), ethyl bromoacetate (12.02 g, 72 mmol) and anhydrous potassium carbonate (10.9 g, 79.2 mmol) in 250 ml of dry 2-butanone is heated at 80° C. for 20 hours. After cooling, the inorganic salts are filtered off and the filtrate is reduced to approximately 120 ml. After addition of cold t-butyl methyl ether the resulting precipitate is filtered off, rinsed with cold t-butyl methyl ether and dried to give 8.6 g of 3-(ethoxycarbonylmethoxy)picolinamide (53%).

WORKUP

后处理

  1. temperatureAfter cooling
  2. filtrationthe inorganic salts are filtered off
  3. additionAfter addition of cold t-butyl methyl ether the resulting precipitate
  4. filtrationis filtered off
  5. washrinsed with cold t-butyl methyl ether
  6. customdried