反应详情

To a stirred suspension of LAH (0.9 g, 25.9 mmol) in dry THF (150 mL) was added 1,4-dibenzyl-piperazine-2-carboxylic acid amide (4.0 g, 12.93 mmol) and the mixture was stirred under reflux for 20 h (monitored by TLC). The stirred mixture was cooled with an ice-bath and quenched with Rochelle's salt (6 mL), warmed to room temperature, and the suspension was poured over a pad of silica gel (20 mm). The celite was washed with 15% MeOH in CH2Cl2 with 1% NH4OH (3×50 mL) and eluted through pad of silica gel. The eluent was concentrated under reduced pressure to give the desired product in 99% yield.

1. temperatureunder reflux for 20 h (monitored by TLC)
2. temperatureThe stirred mixture was cooled with an ice-bath
3. customquenched with Rochelle's salt (6 mL)
4. additionthe suspension was poured over a pad of silica gel (20 mm)
5. washThe celite was washed with 15% MeOH in CH2Cl2 with 1% NH4OH (3×50 mL)
6. washeluted through pad of silica gel
7. concentrationThe eluent was concentrated under reduced pressure