化学合成。
化学合成
合成路线 1(1. 合成:808744-34-5)
产率:78%
合成条件:With sodium hydrogencarbonate In ethanol for 6 h; Reflux
实验步骤:将化合物2-氨基-4-溴吡啶22(5.0g)和2-氯乙醛(40当量溶液,12mL,2.5当量)溶于无水乙醇(50mL)中后加入NaHCO3(4.89g,2.0eq)回流反应6h 通过真空过滤除去有机溶剂,用EA(60mL)洗涤,用水洗涤,用盐水饱和,用Na 2 SO 4干燥并在干燥柱上干燥,得到棕色固体23(4.38g,78%)。
参考文献:
- [1] Patent: CN106496222, 2017, A. Location in patent: Paragraph 0095; 0097 [2] Patent: WO2008/124323, 2008, A1. Location in patent: Page/Page column 68 [3] Patent: WO2008/121687, 2008, A2. Location in patent: Page/Page column 53 [4] Patent: WO2017/144633, 2017, A1. Location in patent: Page/Page column 101; 102 [5] Patent: WO2017/144639, 2017, A1. Location in patent: Page/Page column 87 [6] Patent: WO2009/50183, 2009, A2. Location in patent: Page/Page column 116 [7] Patent: WO2010/108074, 2010, A2. Location in patent: Page/Page column 62-63