Hydrochloric Acid → 4-Amino-1-(4-pyridyl)piperidine trihydrochloride hydrate
反応式
C([NH:4][CH:5]1[CH2:10][CH2:9][N:8]([C:11]2[CH:16]=[CH:15][N:14]=[CH:13][CH:12]=2)[CH2:7][CH2:6]1)(=[O:3])C.[ClH:17]>>[OH2:3].[ClH:17].[ClH:17].[ClH:17].[NH2:4][CH:5]1[CH2:6][CH2:7][N:8]([C:11]2[CH:12]=[CH:13][N:14]=[CH:15][CH:16]=2)[CH2:9][CH2:10]1参加物
3
実験手順
The product from step (iii) (0.52 g) in 1 molar hydrochloric acid (11.9 ml) was heated at 95° C. for 5 hours. The solvent was evaporated and the residue, on drying over potassium hydroxide in vacuo gave 4-amino-1-(4-pyridyl)piperidine trihydrochloride hydrate, 0.70 g as a light brown solid: m.p. >300° C.; NMR (d6DMSO) δ 8.28(4H,m), 7.22(2H,d), 4.27(2H,bd), 3.5 to 3.15(3H+H2O), 2.09(2H,m), 1.59(2H,dq); m/e 178(M+H)+ ; calculated for C10H15N3. 3HCl. 0.75 H2O: C, 40.0; H, 6.5; N, 14.0. found: C, 40.4; H, 6.3; N, 13.5%.
後処理
- customThe solvent was evaporated
- dry with materialthe residue, on drying over potassium hydroxide in vacuo