反应详情

温度

60 °C

Under a nitrogen atmosphere, triethylamine (1.73 ml, 0.01243 mol) and ethyl 5-bromovalerate (1.72 ml, 0.0109 mol) were added to a solution of N-benzylglycine ethyl ester (2.0 g, 0.0103 mol) in acetonitrile (40 ml) at room temperature, and the resulting mixture was heated at 60° C. After 1 hour, the mixture was refluxed. After 9 hours, the mixture was concentrated under reduced pressure, and the resulting residue was extracted with water (200 ml) and ethyl acetate (200 ml×2) and the organic layer was dried over anhydrous magnesium sulfate. The organic layer dried was concentrated under reduced pressure and the resulting residue was purified by a silica gel column chromatography (eluent: hexane/ethyl acetate) to obtain ethyl 5-[benzyl(2-ethoxy-2-oxoethyl)amino]pentanoate (1.2473 g, 37%).

1. temperaturethe mixture was refluxed
2. waitAfter 9 hours
3. concentrationthe mixture was concentrated under reduced pressure
4. extractionthe resulting residue was extracted with water (200 ml) and ethyl acetate (200 ml×2)
5. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
6. customThe organic layer dried
7. concentrationwas concentrated under reduced pressure
8. customthe resulting residue was purified by a silica gel column chromatography (eluent: hexane/ethyl acetate)