反应详情

温度

80 °C

A mixture of 2-isopropyl-4-nitro-benzoic acid (0.23 g, 1.10 mmol), 2-bromoethanol (1.0 mL, 14.1 mmol) and conc. sulfuric acid (0.2 mL) was heated at 80° C. overnight. The mixture was cooled to r.t., diluted with water and extracted twice with ethyl acetate. The organic phase was washed with sat. sodium bicarbonate solution, water and brine then dried over sodium sulfate and concentrated. The crude product was purified by column chromatography on silica (60-120 mesh), eluting with 7% ethyl acetate/petroleum ether, to afford 2-isopropyl-4-nitro-benzoic acid 2-bromo-ethyl ester (0.24 g, 69%) as a colourless oil.

1. temperatureThe mixture was cooled to r.t.
2. extractionextracted twice with ethyl acetate
3. washThe organic phase was washed with sat. sodium bicarbonate solution, water and brine
4. dry with materialthen dried over sodium sulfate
5. concentrationconcentrated
6. customThe crude product was purified by column chromatography on silica (60-120 mesh)
7. washeluting with 7% ethyl acetate/petroleum ether