化学合成。
化学合成
合成路线 1(1. 合成:64436-92-6)
产率:25%
合成条件:at 140℃; for 20 h; Microwave irradiation; Sealed tube
实验步骤:将3-溴-5-甲氧基吡啶(9f5)(500mg,2.66mmol),氢氧化铵(15mL)和五水合硫酸钴(33mg,0.13mmol)在140℃下在微波炉中在密闭管中加热20小时。。 将反应混合物冷却至室温,将粗物质在乙酸乙酯和水之间分离。 将有机层用水(3次)和盐水洗涤,经MgSO 4干燥,过滤并真空浓缩,得到84mg,得到25%的所需产物,为固体。 1H NMR(400MHz,CDCl3):δ7.72(d,J = 5.4Hz,2H),6.51(t,J = 2.4Hz,1H),3.79(s,3H)ppm; HPLC-MS:m / z 125.0
参考文献:
- [1] Organic Process Research and Development, 2012, vol. 16, # 5, p. 788 - 797 [2] Advanced Synthesis and Catalysis, 2013, vol. 355, # 4, p. 627 - 631 [3] European Journal of Medicinal Chemistry, 2015, vol. 106, p. 50 - 59 [4] Patent: US2007/167497, 2007, A1. Location in patent: Page/Page column 26 [5] Patent: US2014/336182, 2014, A1. Location in patent: Paragraph 0315 [6] Patent: WO2008/124083, 2008, A2. Location in patent: Page/Page column 49 [7] Patent: WO2007/113548, 2007, A1. Location in patent: Page/Page column 154