反应详情

温度

80 °C

To a stirred solution of 2-Bromo-N-(2-hydroxy-phenyl)-2-methyl-propionamide (21.8 g, 84.4 mmol) in DMF (85 mL) at 25° C. was added potassium carbonate (23.32 g, 168.99 mmol) and stirred the reaction mixture at 80° C. for 4 h. After TLC reaction mixture was filtered through celite and diluted with ethyl acetate 500 mL and then washed with water (100 mL×3), brine (100 mL), dried over anhydrous sodium sulfate, concentrated to give 2,2-dimethyl-4H-benzo[1,4]oxazin-3-one (12.64 g) as brown solid which was purified by column chromatography to furnish 8.5 g pure compound.

1. filtrationAfter TLC reaction mixture was filtered through celite
2. additiondiluted with ethyl acetate 500 mL
3. washwashed with water (100 mL×3), brine (100 mL)
4. dry with materialdried over anhydrous sodium sulfate
5. concentrationconcentrated