反应详情

温度

140 °C

1-(Bromomethyl)-2,5-difluoro-4-nitrobenzene (8.3 g, 32.9 mmol) and triethyl phosphate (12.03 mL) were heated in an oil bath for 2.5 hours at 140° C. Additional triethyl phosphate (5 mL) was added and the reaction was stirred at 140° C. for 1 hour. The reaction mixture was evaporated under reduced pressure and chromatographed on silica eluting with dichloromethane/methanol (1:0-1%) to give the title compound (11 g, 35.6 mmol). 1H NMR (CDCl3, 400 MHz): δ 7.82 (dd, 1H), 7.37 (ddd, 1H), 4.11 (m, 4H), 3.24 (d, 2H), 1.30 (m, 6H)

1. customThe reaction mixture was evaporated under reduced pressure
2. customchromatographed on silica eluting with dichloromethane/methanol (1:0-1%)