反应详情

2.68 g (14.1 mmol) of ethyl 4,4-dimethoxy-3-oxo-butyrate, 3.62 ml (34.9 mmol) of benzyl alcohol and 244 mg (2.0 mmol) of 4-dimethylaminopyridine were heated under reflux in 40 ml of toluene for three nights. A phosphate buffer solution was added to the obtained reaction solution. 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 evaporated 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. customThe solvent was evaporated under reduced pressure
5. customthe residue was purified by the silica gel chromatography (hexane/ethyl acetate=9:1)