反应详情

A solution of methyl 3-fluoro-4-nitrobenzoate (1.99 g, 10 mmol) and 3-chloro-4-(trifluoromethoxy)aniline (4.23 g, 20 mmol) in dimethylsulfoxide (10 mL) was stirred at 160° C. for 2 days. After cooling, the reaction mixture was diluted with ethyl acetate, washed with water and saturated brine, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=4/1) and recrystallized from hexane/ethyl acetate to give the title compound (1.47 g, yield 38%) as orange crystals.

1. temperatureAfter cooling
2. washwashed with water and saturated brine
3. dry with materialdried over anhydrous magnesium sulfate
4. concentrationconcentrated under reduced pressure
5. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate=4/1)
6. customrecrystallized from hexane/ethyl acetate