反应详情

To a solution of 2,5-dimethyl-3-[4-(phenylmethyl)piperazin-1-yl]pyrazine (Preparation 17, 1.14 g, 4.04 mmol) in methanol (80 ml) was added ammonium formate (1.27 g, 20.2 mmol) followed by palladium (10% w/w on carbon, 0.17 g) under a nitrogen atmosphere. The reaction mixture was heated under reflux, after 2.5 h, more ammonium formate (0.64 g, 10.1 mmol) and palladium (0.06 g) were added. The reaction mixture was filtered through Celite® washed with methanol and concentrated in vacuo. The crude product was purified by flash chromatography using silica gel eluting with methanol:dichloromethane (8:92 and then 10:90) and then methanol:dichloromethane:0.88 ammonia solution (10:90:1). The title compound was obtained as a white solid (0.35 g, 45%).

1. temperatureThe reaction mixture was heated
2. temperatureunder reflux, after 2.5 h
3. filtrationThe reaction mixture was filtered through Celite®
4. washwashed with methanol
5. concentrationconcentrated in vacuo
6. customThe crude product was purified by flash chromatography