反应详情

温度

70 °C

To a 1.0 L flask was added tert-butyl 4-oxopiperidine-1-carboxylate (150.0 g, 752.8 mmol), which was dissolved in DMF (400 mL). To this solution was added TMS-Cl (114.7 mL, 903.4 mmol), followed by NEt3 (251.8 mL, 1807 mmol). The resulting heterogeneous mixture was warmed to 70° C. and stirred overnight under a N2 atmosphere. The mixture was cooled to ambient temperature, diluted with hexanes (250 mL) and filtered. The solids were washed with hexanes (4×250 mL). The combined organic phases were washed with a saturated aqueous NaHCO3 (3×250 mL) and brine (3×250 mL), dried over Na2SO4, and concentrated. The crude product was carried on directly to the next step.

1. temperatureThe mixture was cooled to ambient temperature
2. filtrationfiltered
3. washThe solids were washed with hexanes (4×250 mL)
4. washThe combined organic phases were washed with a saturated aqueous NaHCO3 (3×250 mL) and brine (3×250 mL)
5. dry with materialdried over Na2SO4
6. concentrationconcentrated