反应详情

温度

80 °C

A mixture of tert-butyl 7-oxa-3-azabicyclo[4.1.0]heptane-3-carboxylate (5.46 g, 27.4 mmol) and triethylamine trihydrofluoride (4.42 g, 27.4 mmol) in DCE (4 mL) was stirred at 80° C. (bath) for 18 hours. After cooling to room temperature, saturated sodium bicarbonate (20 mL) and DCM (30 mL) were added. The organic phase was separated, washed with brine, dried (sodium sulfate) and concentrated in vacuo. The residue obtained was purified by flash chromatography on silica gel (hexane:ethyl acetate 1:1) to give trans-tert-butyl 4-fluoro-3-hydroxypiperidine-1-carboxylate (3.5 g, 58%) as a solid.

1. temperatureAfter cooling to room temperature
2. customThe organic phase was separated
3. washwashed with brine
4. dry with materialdried (sodium sulfate)
5. concentrationconcentrated in vacuo
6. customThe residue obtained
7. customwas purified by flash chromatography on silica gel (hexane:ethyl acetate 1:1)