反应详情

温度

0 °C

To a solution of 2-[1-(3-tert-butoxycarbonylamino-propyl)piperidin-4-yl] benzonitrile (0.73 g, 2.1 mmol) in ethyl acetate (100 ml), cooled to 0° C. was added hydrogen chloride gas, bubbled vigorously for 5 minutes. The reaction mixture was stirred for 10 minutes at 0° C., purged with argon and concentrated. Flushing with ethyl acetate×2 and concentration gave 2-[1-(3-arninopropyl)-piperidin4-yl] benzonitrile hydrochloride; 1H NMR (DMSO) d 2.00 (m, 2H), 2.10 (m, 2H), 2.28 (m, 2H), 2.95 (m, 2H), 3.18 (m, 4H), 3.56 (bd, 2H, J=11.7 Hz), 7.47 (m, 2H), 7.75 (bt, 1H, J=8 Hz), 7.84 (bd, 1H, J=7.9 Hz), 8.14 (bs, 2H), 11.1 (bd, 1H).

1. custombubbled vigorously for 5 minutes
2. custompurged with argon
3. concentrationconcentrated
4. customFlushing with ethyl acetate×2 and concentration