反应详情

A solution of 3-fluoro-4-methoxybenzaldehyde (2.20 g, Ald) in 1,2-diethoxyethane (5 ml) was added with ethyl diethylphosphonoacetate (3.12 ml, TCI) and added with 60% sodium hydride (624 mg) under ice cooling. After being stirred for 10 minutes, the reaction mixture was warmed to room temperature, and stirred for 5 hours. The reaction mixture was added with ethyl acetate (90 ml), and washed successively with saturated aqueous sodium hydrogencarbonate, saturated aqueous ammonium chloride and saturated brine. The organic layer was dried, and then the solvent was evaporated under reduced pressure. The residue was purified by flash column chromatography (Quad, hexane:ethyl acetate=10:1) to obtain the title compound (Intermediate 7, 3.16 g).

1. stirringstirred for 5 hours
2. washwashed successively with saturated aqueous sodium hydrogencarbonate, saturated aqueous ammonium chloride and saturated brine
3. customThe organic layer was dried
4. customthe solvent was evaporated under reduced pressure
5. customThe residue was purified by flash column chromatography (Quad, hexane:ethyl acetate=10:1)