化学合成。
化学合成
合成路线 1(1. 合成:1220220-21-2)
产率:91.1%
合成条件:With (1,1'-bis(diphenylphosphino)ferrocene)palladium(II) dichloride; potassium acetate In 1,4-dioxane at 100℃; Inert atmosphere; Industrial scale
实验步骤:向装有磁力搅拌器,温度计,回流冷凝器和鼓泡器的1L四颈烧瓶中加入55.91g(0.26mol)2-乙酰氨基-4-溴吡啶,66.02g(0.26mol)双(频率峰)。 )加入diboron和76.44g(0.78mol),加入450mL二恶烷并搅拌。 在氮气氛下,加入3.81g(0.0051mol)二茂铁氯化钯,温度至100℃反应18至24小时,TLC控制至反应结束,温度为沉淀固体,打浆过滤,加入甲醇500mL溶解,过滤 蒸发至干,加庚烷打浆,得到产物62.08g,收率91.1%。
参考文献:
- [1] Patent: CN103601745, 2017, B. Location in patent: Paragraph 0025; 0026 [2] Angewandte Chemie - International Edition, 2016, vol. 55, # 36, p. 10890 - 10894 [3] Angew. Chem., 2016, vol. 128, p. 11050 - 11054,5 [4] Journal of Medicinal Chemistry, 2017, vol. 60, # 13, p. 5613 - 5637 [5] Patent: US2013/165464, 2013, A1. Location in patent: Paragraph 0835 [6] Patent: WO2015/108881, 2015, A1. Location in patent: Paragraph 00116 [7] Patent: WO2015/108861, 2015, A1. Location in patent: Paragraph 00180 [8] Patent: US2015/225422, 2015, A1. Location in patent: Paragraph 0235; 0237 [9] Patent: US2016/333007, 2016, A1. Location in patent: Paragraph 0227