反应详情

To 10.0 g of 4-(1-benzyl-4-hydroxypiperidin-4-yl)-2-methoxybenzaldehyde dimethyl acetal were added 100 ml of toluene and 6.15 g of p-toluenesulfonic acid monohydrate and the resulting mixture was heated under reflux for 1 hour. To the reaction mixture were added water and triethylamine followed by extraction with ethyl acetate. The organic layer was washed with water and a saturated aqueous solution of sodium chloride and dried over anhydrous sodium sulfate. After distilling off the solvent under reduced pressure, the residue was purified by silica gel column chromatography (eluted with dichloromethane/methanol) to thereby give 3.43 g of the title compound as a pale brown oily substance.

1. temperaturethe resulting mixture was heated
2. temperatureunder reflux for 1 hour
3. extractionfollowed by extraction with ethyl acetate
4. washThe organic layer was washed with water
5. dry with materiala saturated aqueous solution of sodium chloride and dried over anhydrous sodium sulfate
6. distillationAfter distilling off the solvent under reduced pressure
7. customthe residue was purified by silica gel column chromatography (eluted with dichloromethane/methanol)