反应详情

To a 30° C. solution of 6-amino-4-methyl-2,10-dihydro-9-oxa-1,2,4a-triaza-phenanthren-3-one (Preparation #2, Step E, 3.0 g, 12.92 mmol) in MeOH (15 mL) and DCM (7.5 mL) was added tetrabutylammonium tribromide (3.31 g, 12.92 mmol) in portions and the resulting black solution was stirred for 1 h. The solvent was removed in vacuo and the residue was purified by column chromatography on silica gel (eluting with 1-50% EtOAc in petroleum ether) to give 6-amino-7-bromo-4-methyl-2,10-dihydro-9-oxa-1,2,4a-triaza-phenanthren-3-one (1.2 g, 3.86 mmol, 30%). LC/MS (Table 1, Method 4) Rt=1.337 min.; MS m/z: 311/313 [M+H]+.

1. customThe solvent was removed in vacuo
2. customthe residue was purified by column chromatography on silica gel (eluting with 1-50% EtOAc in petroleum ether)