反应详情

Under nitrogen atmosphere, to a suspension of lithium aluminum hydride (0.85 g) in tetrahydrofuran (65 ml) was added (3R)-1-benzyl-3-(4-methoxybenzyl)piperazine-2,5-dione (3.65 g) portionwise under ice-bath cooling. The reaction mixture was refluxed with stirring for one hour. After cooling, it was quenched by sequential addition of water (0.85 ml), 15% aqueous sodium hydroxide (0.85 ml), and water (2.5 ml) and the whole was stirred at room temperature for 30 minutes. The resulting insoluble material was removed by filtration, and the filtrate was added to a mixture of ethyl acetate (50 ml) and brine (70 ml). The organic layer was separated, dried over magnesium sulfate, and concentrated under reduced pressure to give (2R)-2-(4-methoxybenzyl)-4-benzylpiperazine (3.51 g) as a syrup.

1. temperaturecooling
2. temperatureThe reaction mixture was refluxed
3. temperatureAfter cooling
4. customit was quenched by sequential addition of water (0.85 ml), 15% aqueous sodium hydroxide (0.85 ml), and water (2.5 ml)
5. stirringthe whole was stirred at room temperature for 30 minutes
6. customThe resulting insoluble material was removed by filtration
7. additionthe filtrate was added to a mixture of ethyl acetate (50 ml) and brine (70 ml)
8. customThe organic layer was separated
9. dry with materialdried over magnesium sulfate
10. concentrationconcentrated under reduced pressure