路线1:以4-(嘧啶-2-基)哌啶-1-羧酸叔丁酯为原料
- 原料:4-(嘧啶-2-基)哌啶-1-羧酸叔丁酯(4.64 g,17.6 mmol)、4N HCl的二恶烷溶液(50 mL)
- 步骤:将原料溶于4N HCl的二恶烷溶液中,室温搅拌2.25小时;反应完成后浓缩混合物,得到产物(无需进一步纯化)
- 收率:100%
- 产物表征:1H NMR(500 MHz,CD3OD)δ 8.95(d,J = 5.5 Hz,2H),7.60(t,J = 5.0 Hz,1H),3.53(dt,J = 13.0, 3.5 Hz,2H),3.35(tt,J = 4.0, 11.0 Hz,1H),3.20(br t,J = 13.8 Hz,2H),2.30(br d,J = 14.0 Hz,2H),2.11-2.20(m,2H);ESI-MS计算值C9H13N3 [M+H]+ 163,实测值164(M+H)
- 参考文献:
- [1] Patent: WO2004/41777, 2004, A2. Location in patent: Page 48
- [2] Patent: WO2004/94371, 2004, A2. Location in patent: Page 72
- [3] Patent: US2008/81803, 2008, A1. Location in patent: Page/Page column 31