反应详情

温度

70 °C

To a solution of tert-butyl 3-hydroxypiperidine-1-carboxylate (2.00 g, 9.94 mmol) in chloroform (20 ml) were successively added p-toluenesulfonyl chloride (2.27 g, 11.9 mmol) and triethylamine (1.66 ml, 11.9 mmol) at 0° C., and the mixture was stirred at 70° C. for 9 hr. The reaction mixture was allowed to cool to room temperature, water was added to the reaction mixture and the mixture was extracted with chloroform. The organic layer was successively washed with water and saturated brine and dried over anhydrous magnesium sulfate. After filtration, the solvent was concentrated under reduced pressure, and the residue was purified by silica gel chromatography (ethyl acetate:hexane=1:1) to give tert-butyl 3-(toluene-4-sulfonyloxy)piperidine-1-carboxylate (1.00 g, yield 28%).

1. customat 0° C.
2. temperatureto cool to room temperature
3. extractionthe mixture was extracted with chloroform
4. washThe organic layer was successively washed with water and saturated brine
5. dry with materialdried over anhydrous magnesium sulfate
6. filtrationAfter filtration
7. concentrationthe solvent was concentrated under reduced pressure
8. customthe residue was purified by silica gel chromatography (ethyl acetate:hexane=1:1)