HRID35580

反应详情

EQUATION

反应方程式

HRID 35580 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To a solution of 4-ethyl-2-hydroxy-5-nitrohexanamide (0.36 g) in acetic acid (5 ml) was added chromium trioxide (0.23 g). The resulting mixture was heated at 100° C. for 40 minutes with stirring. After cooling, the mixture was evaporated to dryness. The resulting residue was diluted with water and then extracted with ethyl acetate. The extract was washed successively with water, an aqueous sodium bicarbonate and brine, and then dried over magnesium sulfate. The solvent was removed by distillation to give an oil. The oil was purified by a preparative thin layer chromatography [solvent: methanol-chloroform (5:95)] to give 4-ethyl-5-nitro-2-oxo-hexanamide (50 mg).

WORKUP

后处理

  1. temperatureAfter cooling
  2. customthe mixture was evaporated to dryness
  3. additionThe resulting residue was diluted with water
  4. extractionextracted with ethyl acetate
  5. washThe extract was washed successively with water
  6. dry with materialan aqueous sodium bicarbonate and brine, and then dried over magnesium sulfate
  7. customThe solvent was removed by distillation
  8. customto give an oil
  9. customThe oil was purified by a preparative thin layer chromatography [solvent: methanol-chloroform (5:95)]