反应详情

To a solution of 3-bromo-2-methylaminomethyl-phenylamine (1.153 g, 5.36 mmol) in CH2Cl2 (50 ml) was added NEt3 (1.5 ml, 10.76 mmol), triphosgen (555 mg, 1.87 mmol) at 0° C. The reaction was allowed to warm up to room temperature and stirred overnight. After the solvent was removed by using a rotary evaporator, the residue was partitioned between water and ethyl acetate. The organic layer was washed by H2O and brine. After drying over MgSO4, the organic fraction was concentrated in vacuo and resulting brown residue was purified by flash chromatography to give 5-bromo-3-methyl-3,4-dihydro-1H-quinazolin-2-one as white solid. (650 mg, 50%) MS: (M+H)+241.1.

1. customAfter the solvent was removed
2. customa rotary evaporator
3. customthe residue was partitioned between water and ethyl acetate
4. washThe organic layer was washed by H2O and brine
5. dry with materialAfter drying over MgSO4
6. concentrationthe organic fraction was concentrated in vacuo
7. customresulting brown residue
8. customwas purified by flash chromatography