HRID858960

反应详情

EQUATION

反应方程式

HRID 858960 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturethe mixture was refluxed
  2. temperatureunder heating for 5 h
  3. customEthanol was evaporated by concentration under reduced pressure and ethyl acetate (50 ml)
  4. additionwas added
  5. washThe mixture was washed with water (20 ml) and saturated brine (20 ml)
  6. customEthyl acetate was evaporated by concentration under reduced pressure
  7. customthe residue was purified by silica gel column chromatography