反应详情

温度

60 °C

To a solution of methyl (2S)-5-pyrrolidone-2-carboxylate (80 g) in tetrahydrofuran (900 ml) was added sodium hydride (60% in oil, 23.5 g) by portions. After the addition, the reaction mixture was heated to 60° C., and benzyl bromide (69.8 ml) was added dropwise thereto. After 3 hours, the reaction mixture was cooled to room temperature and water (100 ml) was added dropwise thereto. The reaction mixture was poured into a mixture of ethyl acetate (2 l) and water (800 ml). The organic layer was separated, washed with brine, and dried over magnesium sulfate. Evaporation of the solvent gave an oil, which was chromatographed on silica gel (2 l) eluting with a mixture of hexane and ethyl acetate (1:1→1:2, V/V) to give methyl (2S)-1-benzyl-5-pyrrolidone-2-carboxylate (100.8 g).

1. additionAfter the addition
2. temperaturethe reaction mixture was cooled to room temperature
3. customThe organic layer was separated
4. washwashed with brine
5. dry with materialdried over magnesium sulfate
6. customEvaporation of the solvent
7. customgave an oil, which
8. customwas chromatographed on silica gel (2 l)
9. washeluting with a mixture of hexane and ethyl acetate (1:1→1:2, V/V)