反应详情

温度

60 °C

A mixture of 4-amino-2-methyl-3-nitrobenzoic acid (synthesized in reagent preparation 22, step 1) (500 mg, 2.6 mmol) methanol (25 mL) and concentrated sulfuric acid (1.25 mL) was stirred at 60° C. for 18 hours. The reaction mixture was cooled concentrated, diluted with ethyl acetate (50 mL), washed with water (50 mL), saturated aqueous sodium bicarbonate solution (2×30 mL), brine (30 mL), dried over sodium sulfate, filtered and concentrated to give the methyl 4-amino-2-methyl-3-nitrobenzoate (400 mg, 75% yield), MS (EI) for C9H10N2O4: 211 (MH+).

1. temperatureThe reaction mixture was cooled
2. concentrationconcentrated
3. additiondiluted with ethyl acetate (50 mL)
4. washwashed with water (50 mL), saturated aqueous sodium bicarbonate solution (2×30 mL), brine (30 mL)
5. dry with materialdried over sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated