反应详情

In DMF (20 ml), 5-fluoro-3-methoxy-2-nitrophenol (4.14 g, 22.1 mmol), benzyl bromide (3.2 ml, 26.5 mmol) and potassium carbonate (4.58 g, 33.2 mmol) were stirred at 70° C. for 5 hours. The reaction mixture was poured in water (200 ml), followed by extraction with ethyl acetate (300 ml). The extract was washed with saturated brine (200 ml), dried over anhydrous magnesium sulfate and distilled under reduced pressure to remove the solvent. The residue was purified by chromatography on a silica gel column, whereby from hexane-ethyl acetate (4:1) eluate fractions, the title compound (6.13 g, 100%) was obtained as a yellow oil.

1. extractionfollowed by extraction with ethyl acetate (300 ml)
2. washThe extract was washed with saturated brine (200 ml)
3. dry with materialdried over anhydrous magnesium sulfate
4. distillationdistilled under reduced pressure
5. customto remove the solvent
6. customThe residue was purified by chromatography on a silica gel column, whereby from hexane-ethyl acetate (4:1) eluate fractions