反应详情

温度

60 °C

A mixture of 2-bromo-4-nitrophenol (Description 6; 14 g, 68.6 mmol), benzyl bromide (14.1 g, 82.4 mmol) and potassium carbonate (47.3 g, 0.343 mol) in dimethylformamide (100 ml) was heated at 60° C. for 3 hours. The mixture was cooled to room temperature and poured into a mixture of ethyl acetate and water. The organic phase was washed with water (3 times) and saturated brine, dried (MgSO4) and the solvent was evaporated under reduced pressure. The residue was recrystallized from methanol to give the title compound (19 g). H NMR (250 MHz, CDCl3) δ 8.48 (1H, d, J 2.8 Hz), 8.18 (1H, dd, J 9.08 Hz, 2.8 Hz), 7.46−7.3 (5H, m), 7.0 (1H, d, J 9.2 Hz), and 5.27 (2H, s).

1. temperatureThe mixture was cooled to room temperature
2. washThe organic phase was washed with water (3 times) and saturated brine
3. dry with materialdried (MgSO4)
4. customthe solvent was evaporated under reduced pressure
5. customThe residue was recrystallized from methanol