反应详情

温度

0 °C

Dissolve tert-butyl-(3R,4R)-4-(4-fluorophenyl)-3-hydroxy-piperidine-1-carboxylate (496 mg, 1.51 mmol) in THF (3 mL) and cool to 0° C. in an ice water bath. Add sodium hydride (84.6 mg, 2.12 mmol), stir for 30 min, and then add methyl iodide (141 uL, 2.27 mmol). Warm to ambient temperature and stir for 5 hours. Quench the reaction with water (5 mL) and separate layers. Extract aqueous layer three times with methyl tert-butyl ether (8 mL), combine organic extracts; dry over magnesium sulphate; filter; collect the filtrate; and concentrate under vacuum to give the title product as a yellow oil (525 mg, 99.9%). MS (m/z): 210 (M+1-Boc).

1. temperatureWarm to ambient temperature
2. customQuench
3. customthe reaction with water (5 mL)
4. customseparate layers
5. dry with materialdry over magnesium sulphate
6. filtrationfilter
7. customcollect the filtrate
8. concentrationand concentrate under vacuum