反应详情

To a solution of 7-benzyloxy-4-methyl-6-nitro-2,10-dihydro-9-oxa-1,2,4a-triaza-phenanthren-3-one (0.14 g, 0.38 mmol) in MeOH (10 mL) was added Raney-Ni (0.03 g). Then the mixture was stirred under an atmosphere of H2 (1 atm) at rt for 2 h. The reaction mixture was filtered and washed with 10% MeOH/DCM (3×10 mL). The filtrate was concentrated in vacuo to give 6-amino-7-benzyloxy-4-methyl-2,10-dihydro-9-oxa-1,2,4a-triaza-phenanthren-3-one (0.065 g, 54%), which was used in the next step directly without further purification. TLC (eluting with 50% EtOAc in petroleum ether) Rf=0.3.

1. filtrationThe reaction mixture was filtered
2. washwashed with 10% MeOH/DCM (3×10 mL)
3. concentrationThe filtrate was concentrated in vacuo