HRID1075457

反应详情

EQUATION

反应方程式

HRID 1075457 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
127.5 °C

PROCEDURE

实验过程

A mixture of 1a (0.5g, 2.4mmol) and 2a (0.41g, 2.4mmol) in N-methyl-2-pyrrolidone (2.5ml) is heated to 120-135° C. for 2 days. After cooling water and diluted sodium hydroxide is added and the mixture is extracted with ethyl acetate. The extract is dried over sodium sulfate, and the solvent is evaporated to leave crude 3a. This crude product is purified by column-chromatography on silica gel using dichloromethane and subsequently a mixture of dichloromethane and methanol (9:1) as the eluents to yield pure 3a (0.61g, 71%) as an oil.

WORKUP

后处理

  1. additionis added
  2. extractionthe mixture is extracted with ethyl acetate
  3. dry with materialThe extract is dried over sodium sulfate
  4. customthe solvent is evaporated