Hydrogen chloride-ethyl acetate → 3-[2-(4-Piperidinyl)ethyl]benzamide hydrochloride
反応式
[NH2:1][C:2]([C:4]1[CH:5]=[C:6]([CH2:10][CH2:11][CH:12]2[CH2:17][CH2:16][N:15](C(OC(C)(C)C)=O)[CH2:14][CH2:13]2)[CH:7]=[CH:8][CH:9]=1)=[O:3].[ClH:25].CCOC(C)=O>CCOC(C)=O>[ClH:25].[NH:15]1[CH2:16][CH2:17][CH:12]([CH2:11][CH2:10][C:6]2[CH:5]=[C:4]([CH:9]=[CH:8][CH:7]=2)[C:2]([NH2:1])=[O:3])[CH2:13][CH2:14]1参加物
4
実験手順
Tert-butyl 4-{2-[3-(aminocarbonyl)phenyl]ethyl}-1-piperidinecarboxylate (13.8 g) was dissolved in EtOAc (200 ml), and 4 M hydrogen chloride/EtOAc solution (130 ml) was added thereto, followed by stirring at room temperature for 4 hours, and then concentrated. Acetonitrile was added to the resulting residue, followed by heating, and the precipitated crystal was collected by filtration, washed with EtOAc, and dried under reduced pressure to obtain 3-[2-(4-piperidinyl)ethyl]benzamide hydrochloride (11.2 g).