HRID1744020
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
20% Sodium ethoxide (3.74 g, 11 mmol) and diethyl 2-acetamidomalonate (2.39 g, 11 mmol) were dissolved in ethanol (10 ml). A solution of 4-methyl-4-nitropentyl iodide (2.57 g, 10 mmol) in ethanol (8 ml) was added and the mixture was refluxed under heating for 5 h. Ethanol was evaporated by concentration under reduced pressure and ethyl acetate (50 ml) was added. The mixture was washed with water (20 ml) and saturated brine (20 ml). Ethyl acetate was evaporated by concentration under reduced pressure and the residue was purified by silica gel column chromatography to give the objective compound (2.89 g, yield 83.4%).
WORKUP
后处理
- temperaturethe mixture was refluxed
- temperatureunder heating for 5 h
- customEthanol was evaporated by concentration under reduced pressure and ethyl acetate (50 ml)
- additionwas added
- washThe mixture was washed with water (20 ml) and saturated brine (20 ml)
- customEthyl acetate was evaporated by concentration under reduced pressure
- customthe residue was purified by silica gel column chromatography