反应详情

温度

85 °C

3-(3-Fluorophenyl)piperidine hydrochloride a2-4 (432 mg, 2 mmol, 1 eq) and K2CO3 (829 mg, 6 mmol, 3 eq) are added to a solution 2-[2-(2-oxopiperidin-1-yl)phenyl]ethyl 4-methylbenzenesulfonate a2-3 (747 mg, 2 mmol, 1 eq) in acetonitrile (10 ml). The reaction mixture is stirred at 85° C. overnight, then filtered and the filtrate is condensed under reduced pressure. The residue is purified by basic reverse phase chromatography over silicagel (gradient CH3CN/H2O/NH4OH from 50/50/0.1 to 80/20/0.1) to afford 472 mg (1.24 mmol) of 1-(2-{2-[3-(3-fluorophenyl)piperidin-1-yl]ethyl}phenyl)piperidin-2-one as a free base. Oxalic acid (111 mg, 1.24 mmol, 1 eq) is added to the residue dissolved in diethylether. The precipitate obtained is filtered and dried under vacuum to afford 517 mg of 1-(2-{2-[3-(3-fluorophenyl)piperidin-1-yl]ethyl}phenyl)piperidin-2-one oxalate 24.

1. filtrationfiltered
2. customcondensed under reduced pressure
3. customThe residue is purified by basic reverse phase chromatography over silicagel (gradient CH3CN/H2O/NH4OH from 50/50/0.1 to 80/20/0.1)