反应详情

To ethyl diethylphosphonoacetate (24.7 g) was added THF (200 ml), and sodium hydride (60%, 4.4 g) was added at 0° C. to the resulting mixture, to which was then added dropwise a solution of 3-propoxybenzaldehyde (16.1 g) in THF (100 ml). The resulting mixture was stirred at room temperature for 1.5 hours. The reaction mixture was poured into water, was neutralized with hydrochloric acid and was extracted with ethyl acetate. The organic layer was washed with an aqueous saturated solution of sodium chloride and was dried with anhydrous magnesium sulfate. After concentration under reduced pressure to remove the solvent, the residue was purified by silica gel column chromatography (hexane:ethyl acetate=6:1) to obtain ethyl 3-propoxycinnamate (24.0 g) as a yellow oil.

1. additionwas added at 0° C. to the resulting mixture, to which
2. extractionwas extracted with ethyl acetate
3. washThe organic layer was washed with an aqueous saturated solution of sodium chloride
4. dry with materialwas dried with anhydrous magnesium sulfate
5. concentrationAfter concentration under reduced pressure
6. customto remove the solvent
7. customthe residue was purified by silica gel column chromatography (hexane:ethyl acetate=6:1)