HRID503748
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customthe phases separated
- extractionthe aqueous layer extracted twice with dichloromethane
- dry with materialthe combined organic layers are dried over Na2SO4
- concentrationconcentrated