反应详情

Lithium aluminium hydride (1.6 g, 42.16 mmol) was added in portions to a stirred mixture of (S)-2-benzylpiperazine-3,6-dione (3.0 g, 14.70 mmol) and tetrahydrofuran (80 ml) at 0° C. After 30 min at ice-bath temperature, the mixture was refluxed for 4 h with stirring. The reaction was quenched by the portionwise addition of sodium sulfate decahydrate and some methanol until hydrogen evolution ceased. It was filtered and the solids were washed several times with dichloromethane. The combined filtrates were evaporated to leave a white solid. MS (m/z): 177.1 (M+H)+; C11H16N2 requir. 176.3.

1. temperaturethe mixture was refluxed for 4 h
2. customThe reaction was quenched by the portionwise addition of sodium sulfate decahydrate
3. filtrationIt was filtered
4. washthe solids were washed several times with dichloromethane
5. customThe combined filtrates were evaporated
6. customto leave a white solid