反应详情

To a solution of crude 2-chloro-4-difluoromethoxy-3-dimethoxymethyl-1-fluorobenzene (181 g, 670 mmol) in acetone (650 mL) and water (150 mL) was added Amberlyst-15 resin (540 g, pre-washed with water) and the mixture was stirred using mechanical stirrer for 40 h at RT. The Amberlyst-15 resin was removed by filtration using celite bed on sintered funnel, and the filtrate was evaporated on a rotary evaporator at RT (Note: aldehyde evaporates at higher temperatures under reduced pressure). The residue was purified by column chromatography on silica gel using ethyl acetate/hexanes (5% to 10%) to obtain the title compound (60 g, 40%).

1. customfor 40 h
2. customat RT
3. customThe Amberlyst-15 resin was removed by filtration
4. customthe filtrate was evaporated on a rotary evaporator at RT
5. custom(Note: aldehyde evaporates at higher temperatures under reduced pressure)
6. customThe residue was purified by column chromatography on silica gel