反应详情

温度

0 °C

To a solution of 3,5-difluoroanisole (30 g, 208 mmol) in 260 mL dichloromethane was added HNO3 (>90% fuming, 60 mL) dropwise at 0° C. The resulting solution was stirred at 0° C. for 3 hours, then washed water. The aqueous phase was extracted with dichloromethane. The organic phase was washed with brine, dried over magnesium sulfate and condensed on a rotavap. The residue was recrystallized in hexane and ethyl acetate to provide 28.5 g (72% yield) of 1,5-difluoro-3-methoxy-2-nitrobenzene as an off-white powder. 1H NMR (400 MHz, DMSO) δ ppm 7.20 (m, 2H), 3.91 (s, 3H).

1. extractionThe aqueous phase was extracted with dichloromethane
2. washThe organic phase was washed with brine
3. dry with materialdried over magnesium sulfate and condensed on a rotavap
4. customThe residue was recrystallized in hexane