HRID2351579
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
PROCEDURE
实验过程
To a solution of 48 mg (2.1 mmol) of sodium in 40 ml of methanol is added 2.0 mg (11.8 mmol) of 5-amino-3-ethoxycarbonyl-1-methylpyrazole, and the mixture is refluxed over night, and distilled under reduced pressure. To the resulting residue are added a small amount of water and sodium chloride, and the mixture is extracted 6 times with chloroform. The extract is dried with magnesium sulfate, chromatographed on a column of silica gel and eluted with ethyl acetate to give 1.37 g (74.1% yield) of the objective compound.
WORKUP
后处理
- temperaturethe mixture is refluxed over night
- distillationdistilled under reduced pressure
- additionTo the resulting residue are added a small amount of water and sodium chloride
- extractionthe mixture is extracted 6 times with chloroform
- dry with materialThe extract is dried with magnesium sulfate
- customchromatographed on a column of silica gel
- washeluted with ethyl acetate