路线1:Suzuki偶联反应合成2-氨基-3-苯基吡啶
- 原料:2-氨基-3-溴吡啶(3mmol,0.5g);苯硼酸(4.5或9.0mmol,1.5或3当量);四(三苯基膦)钯(0)(1mol%);磷酸钾(6mmol,2当量);乙二醇(5mL);水(2mL)
- 反应条件:惰性气氛下,80℃加热16小时
- 后处理步骤:反应完成后用1M氢氧化钠溶液(20mL)水解;水相用乙酸乙酯(3×30mL)萃取;合并的有机层用饱和氯化钠溶液(50mL)洗涤,无水硫酸镁干燥,过滤后减压浓缩
- 纯化方法:硅胶柱色谱法,洗脱剂为石油醚/乙酸乙酯(60/40,v/v)
- 产率:80%
- 参考文献:
[1] Chemistry - A European Journal, 2013, vol.19, #28, p.9137-9141
[2] Bioorganic and Medicinal Chemistry Letters, 2016, vol.26, #1, p.114-120
[3] Bioorganic and Medicinal Chemistry Letters, 2017, vol.27, #4, p.911-917
[4] Patent: WO2011/17342, 2011, A2. Location in patent: Page/Page column 116
[5] Patent: WO2015/148344, 2015, A2. Location in patent: Page/Page column 60
[6] Journal of Organic Chemistry, 2016, vol.81, #18, p.8520-8529
[7] Patent: WO2016/161572, 2016, A1. Location in patent: Page/Page column 58; 59
[8] Patent: WO2017/112576, 2017, A1. Location in patent: Paragraph 0035-0036