化学合成。
化学合成
合成路线 1(1. 合成:887707-25-7)
产率:63%
合成条件:at 100℃;
实验步骤:步骤B. 2-氯-5-碘-3-(三氟甲基)二吡啶将5-碘-3-(三氟甲基)吡啶-2-醇(3.0g,10.4mmol)在POCl 3(8mL)中的悬浮液加热至 100°C过夜。 冷却至室温后,将混合物倒入冰(50g)中。 将得到的水层用Na 2 CO 3中和,并用乙酸乙酯(70mL×2)萃取。 合并萃取物,用硫酸钠干燥,过滤,并减压浓缩。 通过硅胶色谱法纯化残余物,使用石油醚:EtOAc(100:1-4:1)作为洗脱溶剂,得到2-氯-5-碘-3-(三氟甲基)吡啶,为白色固体(2.0g,63%))。 1 H NMR(500MHz,CDCl 3)δ(ppm)8.78(d,J = 2.0Hz,1H),8.28(d,J = 2.0Hz,1H)。
参考文献:
- [1] Patent: WO2015/100613, 2015, A1. Location in patent: Page/Page column 17; 18 [2] Patent: WO2015/100617, 2015, A1. Location in patent: Page/Page column 36; 37 [3] Patent: WO2008/119015, 2008, A2. Location in patent: Page/Page column 48-49 [4] Patent: JP2016/11315, 2016, A. Location in patent: Paragraph 0084 [5] Patent: US9388159, 2016, B2. Location in patent: Page/Page column 20; 21 [6] Synthetic Communications, 2006, vol. 36, # 9, p. 1235 - 1245 [7] Patent: WO2009/18656, 2009, A1. Location in patent: Page/Page column 53-54 [8] Patent: WO2009/18657, 2009, A1. Location in patent: Page/Page column 63; 64 [9] Patent: WO2009/76747, 2009, A1. Location in patent: Page/Page column 62-63 [10] Patent: WO2011/103202, 2011, A2. Location in patent: Page/Page column 157 [11] Patent: WO2015/196144, A2. Location in patent: Paragraph 0326 [11] Patent: , 2015, . Location in patent: Paragraph 0326 [13] Patent: US2008/45516, 2008, A1. Location in patent: Page/Page column 30