反应详情

温度

40 °C

The anthranilic acid (388 mg, 1.97 mmol) prepared in Example 2 was taken up in anhydrous methylene chloride (10 mL). Triethylamine (2.36 mmol) was added followed by addition of acetic anhydride (2.36 mmol). The reaction mixture was heated at 40° C. for 18 hours. Subsequently, the reaction mixture was poured into water and extracted with methylene chloride. The organic layer was washed with saturated aqueous sodium bicarbonate, brine, dried over magnesium sulfate, filtered, and concentrated in vacuo to afford 5,7-dimethoxy-2-methyl-3,1-benzoxazine-4-one (51% yield).

1. extractionextracted with methylene chloride
2. washThe organic layer was washed with saturated aqueous sodium bicarbonate, brine
3. dry with materialdried over magnesium sulfate
4. filtrationfiltered
5. concentrationconcentrated in vacuo