反应详情

温度

95 °C

To a stirred mixture of 2-bromo-1,4-difluorobenzene (3.24 g, 16.81 mmol) and aluminium chloride (5.82 g, 43.7 mmol) at 60° C. under nitrogen was added dropwise acetyl chloride (1.98 g, 25.28 mmol 1). The mixture was stirred at 95° C. for 1.5 hr and then poured into ice (50 mL). To the mixture was added HCl (3 mL) followed by extraction into ether (20 mL×2). The ether extracts were washed with brine (20 mL) and then concentrated under reduced pressure to obtain the desired crude product (brown oil) as mixture with starting material (55:45) (2.67 g, 33%); 1H NMR (250 MHz, CHLOROFORM-d) delta 2.64 (3H, d, J=5.18 Hz), 7.42 (1H, dd, J=9.44, 5.18 Hz), 7.65 (1H, dd, J=8.45, 6.17 Hz).

1. extractionfollowed by extraction into ether (20 mL×2)
2. washThe ether extracts were washed with brine (20 mL)
3. concentrationconcentrated under reduced pressure