反应详情

2.68 g (14.1 mmol) of ethyl 4,4-dimethoxy-3-oxobutyrate, 5.14 ml (40.0 mmol) of cinnamyl alcohol and 244 mg (2.0 mmol) of 4-dimethylaminopyridine were heated under reflux in 40 ml of toluene for two nights. A phosphate buffer solution was added to the reaction liquid. After the extraction with ethyl acetate, the organic layer was washed with a saturated aqueous salt solution and then dried over anhydrous sodium sulfate. The solvent was distilled under reduced pressure, and the residue was purified by the silica gel chromatography (hexane/ethyl acetate=9/1) to obtain the title compound.

1. extractionAfter the extraction with ethyl acetate
2. washthe organic layer was washed with a saturated aqueous salt solution
3. dry with materialdried over anhydrous sodium sulfate
4. distillationThe solvent was distilled under reduced pressure
5. customthe residue was purified by the silica gel chromatography (hexane/ethyl acetate=9/1)