化学合成。
化学合成
合成路线 1(1. 合成:7627-44-3)
产率:100%
合成条件:With sodium iodide In acetone at 20℃; for 0.58 h; Heating / reflux
实验步骤:将2,4-二氯-5-氯甲基 - 嘧啶(10g,50.6mmol),碘化钠(7.69g,51.3mmol)的丙酮(60ml)混合物在室温下搅拌20分钟,然后回流15分钟。分钟。 使反应冷却至室温,然后过滤固体并用丙酮洗涤。 浓缩滤液,得到2,4-二氯-5-碘甲基 - 嘧啶,为浅黄色固体(14.6g,100%); 1H NMR 400MHz(CDCl3)? 8.54(s,IH),4.33(s,2H); MS m / z 288.9(M + 1)。
参考文献:
- [1] Patent: WO2007/136465, 2007, A2. Location in patent: Page/Page column 43-44 [2] Patent: WO2018/53373, 2018, A1. Location in patent: Paragraph 00485; 00486 [3] Patent: WO2018/160774, 2018, A1. Location in patent: Paragraph 00377; 00378 [4] Patent: WO2018/25043, 2018, A1. Location in patent: Page/Page column 24 [5] Patent: US2016/75720, 2016, A1. Location in patent: Paragraph 0323 [6] Patent: US2004/38995, 2004, A1. Location in patent: Page/Page column 4; 6 [7] Patent: US2004/122029, 2004, A1. Location in patent: Page/Page column 11 [8] Patent: US2004/204427, 2004, A1. Location in patent: Page/Page column 6; 10 [9] Patent: WO2014/144737, 2014, A1. Location in patent: Paragraph 00355 [10] Patent: US2016/115164, 2016, A1. Location in patent: Paragraph 0360 [11] Patent: WO2016/134294, 2016, A1. Location in patent: Paragraph 0229 [12] Patent: WO2016/134314, 2016, A1. Location in patent: Page/Page column 60