With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.138377-80-7,3-Aminopiperidin-2-one hydrochloride,as a common compound, the synthetic route is as follows.
To a solution of 3-aminopiperidin-2-one hydrochloride (1.50 g) in methanol (10 mL) was added AMBERLYST (registered trademark) A21 (750 mg) at room temperature. The reaction mixture was stirred at room temperature overnight, theinsoluble material was removed by filtration, and the filtrate was concentrated under reduced pressure. To a solution of the residue in ethanol (20 mL) was added 4-thioxothiazolidin-2-one (1.330 g) at room temperature. The reaction mixture wasstirred at room temperature overnight, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (NH, methanol/ethyl acetate) . To a solution of the residue and l-[2,4- bis (trifluoromethyl) benzyl] piperidine-4-carbaldehyde (1018 mg) in 2-propanol (10 mL) was added piperidinium acetate (436 mg) at room temperature. The reaction mixture was stirred at 60C overnight, and the solvent was evaporated under reducedpressure. The residue was purified by silica gel columnchromatography (NH, methanol/ethyl acetate) and recrystallized from ethyl acetate/diisopropyl ether to give the titlecompound (530 mg) .? NMR (300 MHz, DMSO-d6) delta 1.38-1.59 (2H, m) , 1.68-1.91 (5H, m) , 2.01-2.27 (4H, m) , 2.69-2.84 (2H, m) , 3.17 (2H, brs) , 3.71 (2H, s), 4.43-4.55 (1H, m) , 6.89 (1H, d, J = 8.8 Hz), 7.83 (1H, brs), 7.98 (1H, s) , 8.02-8.12 (2H, m) , 9.34 (1H, brs).MS (ESI+) : [M+H]+ 535.1., 138377-80-7
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Reference：
Patent; TAKEDA PHARMACEUTICAL COMPANY LIMITED; MATSUMOTO, Shigemitsu; ONO, Koji; TOMINARI, Yusuke; KATOH, Taisuke; MIWA, Kazuhiro; HASUOKA, Atsushi; IMAMURA, Shinichi; WO2013/18929; (2013); A1;,
Piperidine – Wikipedia
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