合成条件:Stage #1: With lithium aluminium tetrahydride In tetrahydrofuran at 23℃; for 3 h; Stage #2: With water; sodium sulfate In tetrahydrofuran for 0.50 h;
实验步骤:E)奎宁环-4-基甲胺/ v NH 2的合成将4-氰基奎宁环(0.30g,2.2mmol)的乙醚(5mL)溶液缓慢加入到LAH(0.167g,4.41mmol)的悬浮液中。在0℃下加入乙醚(15mL)。将反应在23℃下搅拌3小时,然后用硫酸钠十水合物淬灭并再搅拌30分钟。然后加入乙酸乙酯,30分钟后,加入硅藻土,用硅藻土过滤悬浮液。将滤液浓缩至干,得到油状物(0.310g,定量)。该化合物原样用于下一步反应。1 H NMR(400MHz,CDCl 3)δppm:1.31-1.40(6H,m),2.43(2H,s),2.86-2.94(6H,m)。
参考文献:
[1] Patent: WO2008/124757, 2008, A1. Location in patent: Page/Page column 55
[2] Patent: US2013/79319, 2013, A1. Location in patent: Paragraph 0199; 0200
[3] Patent: US5399562, 1995, A
[4] Patent: US6281226, 2001, B1
[5] Patent: US2009/88418, 2009, A1. Location in patent: Page/Page column 20
[6] Bioorganic and Medicinal Chemistry Letters, 2010, vol. 20, # 12, p. 3540 - 3544
[7] Patent: US5821240, 1998, A