路线1:以2-氨基-5-[(三甲基硅基)乙炔基]吡啶为原料合成5-炔吡啶-2-胺
- 原料:5-三甲基硅烷基乙炔基-吡啶-2-基胺(26 mg,137 μmol);碳酸钾(37.9 mg,274 μmol);四氢呋喃(1 mL);甲醇(1 mL);水;乙酸乙酯;饱和氯化钠水溶液;无水硫酸镁
- 步骤:向原料的四氢呋喃和甲醇混合溶液中加入碳酸钾,室温搅拌1小时;反应完成后于0℃分配到水和乙酸乙酯中萃取;有机层用饱和氯化钠水溶液洗涤,无水硫酸镁干燥;减压浓缩除去溶剂,残余物通过硅胶柱色谱(洗脱剂:庚烷/乙酸乙酯=1:1)纯化
- 收率:99%
- 表征:1H-NMR(CDCl3)δ(ppm):3.07(1H,s),4.73(2H,brs),6.46(1H,d,J=8.6 Hz),7.53(1H,dd,J=2.2,8.6 Hz),8.21(1H,s)
- 参考文献:
[1] Patent: US2009/82403, 2009, A1. Location in patent: Page/Page column 76-77
[2] Patent: US2007/105904, 2007, A1. Location in patent: Page/Page column 74
[3] Dalton Transactions, 2006, vol. 6, # 13, p. 1627 - 1635
[4] Patent: WO2005/90333, 2005, A1. Location in patent: Page/Page column 71
[5] Patent: US2007/287739, 2007, A1. Location in patent: Page/Page column 7