反应详情

温度

0 °C

1-t-Butoxycarbonyl-4-methoxy-4-phenylpiperidine (150 mg, 0.51 mmol) was dissolved in a mixed solvent of 1,4-dioxane (20 ml) and concentrated hydrochloric acid (10 ml). The resulting solution was stirred at 0° C. for a while and then gradually returned to a room temperature spending 1.5 hours. The reaction solution was neutralized by adding with sodium hydroxide aqueous solution (1 N), and then the solvent was evaporated under a reduced pressure. The thus obtained residue was mixed with ethyl acetate and water, the reaction product was extracted with ethyl acetate, washed with water and saturated brine and dried with anhydrous sodium sulfate. Then the solvent was evaporated under a reduced pressure was separated and purified by a silica gel column chromatography to obtain 49 mg of the title compound (0.25 mmol, 49% in yield).

1. customgradually returned to a room temperature
2. customthe solvent was evaporated under a reduced pressure
3. additionThe thus obtained residue was mixed with ethyl acetate and water
4. extractionthe reaction product was extracted with ethyl acetate
5. washwashed with water and saturated brine
6. dry with materialdried with anhydrous sodium sulfate
7. customThen the solvent was evaporated under a reduced pressure
8. customwas separated
9. custompurified by a silica gel column chromatography