反应详情

温度

-78 °C

Deoxo-Fluor® was added to a solution of 1,1-dimethylethyl 4-hydroxy-1,4′-bipiperidine-1′-carboxylate (0.500 g, 1.76 mmol) dropwise at −78° C. The mixture was maintained at −78° C. for 30 min before it was warmed to room temperature and stirred for 2 h. The mixture was washed with saturated aqueous sodium bicarbonate. The organic phase was dried over Na2SO4, filtered, and concentrated in vacuo. The crude material was purified via column chromatography (1:200 methanol/methylene chloride) to afford 1,1-dimethylethyl 4-fluoro-1,4′-bipiperidine-1′-carboxylate (0.300 g, 60% yield) as a colorless oil.

1. temperaturewas warmed to room temperature
2. washThe mixture was washed with saturated aqueous sodium bicarbonate
3. dry with materialThe organic phase was dried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customThe crude material was purified via column chromatography (1:200 methanol/methylene chloride)