HRID1580941

反应详情

EQUATION

反应方程式

HRID 1580941 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-30 °C

PROCEDURE

实验过程

A solution of 54.0g of 2-amino-3-methylpyridine, 144.0g of methyl butyrylacetate, 5.0g of p-toluenesulfonic acid, and 750ml of ethylene glycol monomethyl ether is heated in a nitrogen atmosphere, under reflux, for 60 hours. The solution is concentrated to dryness in vacuo, and the residual oil extracted with two 250ml portions of pentane. The pentane solution is concentrated to a volume of 250ml and cooled at -30°C to yield the title compound, melting point 59°-60°C.

WORKUP

后处理

  1. temperatureunder reflux, for 60 hours
  2. concentrationThe solution is concentrated to dryness in vacuo
  3. extractionthe residual oil extracted with two 250ml portions of pentane
  4. concentrationThe pentane solution is concentrated to a volume of 250ml