反应详情

To a solution of 1.0 g of 1-benzyl-4-[4-[2-(methoxymethoxy)ethyl]phenyl]piperidin-4-ol in 30 ml of toluene was added 2.0 g of p-toluenesulfonic acid. Then the resulting mixture was heated under reflux for 1 hour while eliminating the water thus formed with a Dean Stark trap. Then the reaction mixture was brought back to room temperature and a saturated aqueous solution of sodium bicarbonate was added thereto. Then it was extracted with ethyl acetate, washed with a saturated aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate. After distilling off the solvent under reduced pressure, the residue was purified by silica gel column chromatography (eluted with n-hexane/ethyl acetate) to thereby give 0.2 g of the title compound as a brown oily substance.

1. temperatureThen the resulting mixture was heated
2. temperatureunder reflux for 1 hour
3. customthus formed with a Dean Stark trap
4. customwas brought back to room temperature
5. extractionThen it was extracted with ethyl acetate
6. washwashed with a saturated aqueous solution of sodium chloride
7. dry with materialdried over anhydrous magnesium sulfate
8. distillationAfter distilling off the solvent under reduced pressure
9. customthe residue was purified by silica gel column chromatography (eluted with n-hexane/ethyl acetate)