HRID35580
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
- 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
- temperatureAfter cooling
- customthe mixture was evaporated to dryness
- additionThe resulting residue was diluted with water
- extractionextracted with ethyl acetate
- washThe extract was washed successively with water
- dry with materialan aqueous sodium bicarbonate and brine, and then dried over magnesium sulfate
- customThe solvent was removed by distillation
- customto give an oil
- customThe oil was purified by a preparative thin layer chromatography [solvent: methanol-chloroform (5:95)]