反应详情

In 10N NaOH (5.8 ml, 58.0 mmol) and DMSO (20 ml), benzyl 5-fluoro-3-methoxy-2-nitrophenyl ether (5.35 g, 19.3 mmol) was stirred for 15 hours. The reaction mixture was poured in 1N HCl (100 ml), followed by extraction with ether (300 ml). The extract was washed with saturated brine (2×100 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 chloroform-ethyl acetate (4:1) eluate fractions, the title compound (1.43 g, 27%) was obtained as a brown oil.

1. extractionfollowed by extraction with ether (300 ml)
2. washThe extract was washed with saturated brine (2×100 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 chloroform-ethyl acetate (4:1) eluate fractions