反应详情

温度

0 °C

A solution of N-(2-acetyl-phenyl)-acetamide (1 g, 5.65 mmol) in conc. H2SO4 (2.8 mL, 45.2 mmol) was cooled to −20° C. and fuming nitric acid (2 mL, 33 mmol) was slowly added. The reaction mixture was warmed to 0° C. and stirred for 7 h. After completion of the starting material, the reaction mixture was quenched with water and extracted with dichloromethane (2×25 mL). The combined organic layers were washed with brine and water, then dried over anhydrous sodium sulphate and concentrated to dryness. The resulting residue was purified by column chromatography using 1% methanol in chloroform to get the title compound as yellow solid

1. customAfter completion of the starting material, the reaction mixture was quenched with water
2. extractionextracted with dichloromethane (2×25 mL)
3. washThe combined organic layers were washed with brine and water
4. dry with materialdried over anhydrous sodium sulphate
5. concentrationconcentrated to dryness
6. customThe resulting residue was purified by column chromatography