化学合成,医药中间体。
医药; 农药; 化工
合成路线 1(1. 合成:4532-25-6)
产率:89%
合成条件:With sodium hydrogencarbonate In ethanol; water at 20℃; for 20 h; Reflux
实验步骤:7-氯咪唑并[1,2-a]吡啶(化合物65-3)的合成[0000229]向化合物65-2(HCl)的乙醇(15mL)悬浮液中加入碳酸氢钠粉末(3.3g,38.4mmol) ,4当量)和50%氯乙醛水溶液(2.26g,14.4mmol,1.5当量)。 将反应加热回流4小时并在室温下搅拌16小时。 减压浓缩反应物,将残余物溶于水(10mL)和乙酸乙酯(10mL)中。 分离各层,水相用乙酸乙酯(2×5mL)萃取。 合并有机层,用硫酸钠干燥,过滤并浓缩,得到化合物65-3,为深黄色油状物(980mg,收率89%)。
参考文献:
- [1] Bioorganic and Medicinal Chemistry Letters, 2013, vol. 23, # 3, p. 750 - 756 [2] Patent: WO2013/123215, 2013, A2. Location in patent: Paragraph 0000229 [3] Patent: EP2565185, 2013, A1. Location in patent: Paragraph 0114-0115 [4] European Journal of Medicinal Chemistry, 2015, vol. 94, p. 123 - 131 [5] Patent: WO2008/78100, 2008, A2. Location in patent: Page/Page column 93-94 [6] Patent: WO2009/47506, 2009, A1. Location in patent: Page/Page column 110; 111 [7] Patent: WO2009/50183, 2009, A2. Location in patent: Page/Page column 114 [8] Patent: WO2018/136634, 2018, A1. Location in patent: Page/Page column 40; 41 [9] Patent: WO2009/150240, 2009, A1. Location in patent: Page/Page column 101