反应详情

温度

0 °C

To a slurry of lithium aluminum hydride (280 mg, 7.37 mmol) in anhydrous diethyl ether (30 mL) at 0° C., a solution of ethyl N-tert-butoxycarbonyl-4-(4-methylpyridin-2-ylmethyl)piperidine-4-carboxylate (2.7 g, 7.45 mmol) in diethyl ether (20 mL) was added dropwise with the temperature of the reacting mixture maintained below 10° C. The resulting mixture was stirred at 0° C. for 30 min, and quenched with successive addition of water (0.28 mL), 15% aqueous NaOH (0.28 mL), and water (0.84 mL). The resultant slurry was stirred at room temp. for 30 min., and filtered through a small plug of Celite. The filtrate was washed brine, dried over anhydrous magnesium sulfate, and filtered. Concentration of the filtrate under vacuum provided the title alcohol.

1. temperaturemaintained below 10° C
2. customquenched with successive addition of water (0.28 mL), 15% aqueous NaOH (0.28 mL), and water (0.84 mL)
3. stirringThe resultant slurry was stirred at room temp. for 30 min.
4. filtrationfiltered through a small plug of Celite
5. washThe filtrate was washed brine
6. dry with materialdried over anhydrous magnesium sulfate
7. filtrationfiltered