HRID503748

反应详情

EQUATION

反应方程式

HRID 503748 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
180 °C

PROCEDURE

实验过程

A solution of 3.8 g 1,2,4-triazol-3-amine and 6 g ethyl 3-oxo-2-phenylbutanoate is suspended in a mixture of 32 ml DMF and 32 ml N,N-dibutylbutan-1-amine and heated by microwave irradiation to 180° C. for 10 h. The reaction mixture is diluted with water and dichloromethane, the phases separated, the aqueous layer extracted twice with dichloromethane, the combined organic layers are dried over Na2SO4 and concentrated to give the crude product. The crude product is purified by column chromatography (silica gel, dichloromethane/methanol).

WORKUP

后处理

  1. customthe phases separated
  2. extractionthe aqueous layer extracted twice with dichloromethane
  3. dry with materialthe combined organic layers are dried over Na2SO4
  4. concentrationconcentrated