反应详情

Methyl iodide (30.2 g, 213 mmol) was added to a stirred mixture of 3-nitrophthalic acid (15.0 g, 71.0 mmol) and sodium bicarbonate (23.9 g, 284 mmol) in DMF (150 mL) at room temperature, and the mixture was then heated in an oil bath set to 60° C. for 4 hours. The mixture was then poured into 700 mL of ice water. After the ice melted, the mixture was extracted with ethyl acetate (3×150 mL) and the organic phases were washed with water (7×500 mL), dried (MgSO4) and evaporated, providing 16.2 g of the product as a pale yellow solid in 95% yield: 1H NMR (CDCl3) δ 3.95 (s, 3H), 4.02 (s, 3H), 7.69 (t, J=8.1 Hz, 1H), 8.36 (m, 2H).

1. temperaturethe mixture was then heated in an oil bath
2. extractionthe mixture was extracted with ethyl acetate (3×150 mL)
3. washthe organic phases were washed with water (7×500 mL)
4. dry with materialdried (MgSO4)
5. customevaporated