反应详情

温度

50 °C

Protected piperidine 15 (1.2 g, 4.55 mmol) was dissolved in HCl/MeOH (2 M). The reaction mixture was stirred at 50° C. for 2 h. The crude was concentrated under vacuo and was washed with dichloromethane twice. The crude was basified by NaOH solution (6N) to pH 12. The crude was extracted by EtOAc for 6 times. The combined organic layers was evaporated under vacuo yielding final product 16 (724 mg, 3.93 mmol, 86%). H-NMR (DMSO-d6) ∂ 0.78 (q, J=6 Hz, 3H), 0.95 (t, J=5 Hz, 3H), 1.09 (m, 2H), 1.26 (m, 1H), 1.53 (m, 1H), 1.74 (m, 2H), 2.67 (m, 2H), 2.80 (br, 1H), 3.03 (br, 1H), 3.87 (d, J=12 Hz, 1H), 4.23 (br, 1H).

1. concentrationThe crude was concentrated under vacuo
2. washwas washed with dichloromethane twice
3. extractionThe crude was extracted by EtOAc for 6 times
4. customThe combined organic layers was evaporated under vacuo