反应详情

To a suspension of Pd—C (5 wt %, 1.60 g) in methanol (60 ml) was added dropwise a solution of (3RS)-3-benzyloxycarbonylamino-2,3-dihydro-5-isopropyl-1H-1,4-benzodiazepin-2-one (8.00 g) in methanol (60 ml) and then ammonium formate (5.56 g) at room temperature. The reaction mixture was stirred at the same temperature for 1 hour. The catalyst was filtered on Celite®. The filtrate was concentrated in vacuo. The residue was taken up with ethyl acetate (100 ml) and saturated aqueous sodium hydrogen carbonate (100 ml). The organic layer was washed with a brine (100 ml). Dryness over sodium sulfate and evaporation gave (3RS)-3-amino-2,3-dihydro-5-isopropyl-1H-1,4-benzodiazepin-2-one (4.21 g). The product was used in a following reaction step without further purification.

1. customat room temperature
2. filtrationThe catalyst was filtered on Celite®
3. concentrationThe filtrate was concentrated in vacuo
4. washThe organic layer was washed with a brine (100 ml)
5. customDryness over sodium sulfate and evaporation