反应详情

温度

150 °C

The 2-bromo-N-(3-bromo-2-hydroxy-phenyl)-2-methyl-propionamide of step 1 was dissolved in DMF (200 ml), and the DMF solution was added to K2CO3 (6.3 g, 45.58 mmol). The mixture was heated overnight at 150° C., then cooled and poured into a mixture of water/ethyl acetate. The organic fraction was washed with brine. After drying over MgSO4, the organic fraction was concentrated in vacuo and resulting brown residue was purified by flash chromatography to give 8-Bromo-2,2-dimethyl-4H-benzo[1,4]oxazin-3-one as a white solid (84.6%). MS: (M−H)−256.

1. temperaturecooled
2. washThe organic fraction was washed with brine
3. dry with materialAfter drying over MgSO4
4. concentrationthe organic fraction was concentrated in vacuo
5. customresulting brown residue
6. customwas purified by flash chromatography