化学合成。
化学合成
合成路线 1(1. 合成:883500-66-1)
产率:23.3%
合成条件:Stage #1: at -40℃; for 1 h; Stage #2: With ammonium chloride In tetrahydrofuran; water
实验步骤:在-40℃下,将乙烯基溴化镁(300mL的1.0M THF溶液,300mmol)滴加到3-硝基-4-氟 - 溴苯(22g,100mmol)的THF(700mL)溶液中。 在-40℃下1小时后,将混合物用NH 4 Cl水溶液淬灭并用EtOAc萃取。 将有机层经Na 2 SO 4干燥并浓缩,得到粗产物,将其通过硅胶柱色谱法纯化,得到4-溴-7-氟-1H-吲哚(5g,23.3%)。 1H NMRCDCl3400MHzδ6.56-6.58(m,1H),6.72-6.79(m,1H),7.06-7.17(m,1H),7.20-7.24(m,1H),8.45(s,1 H)。
参考文献:
- [1] European Journal of Organic Chemistry, 2006, # 13, p. 2956 - 2969 [2] Patent: WO2013/117522, 2013, A1. Location in patent: Page/Page column 39 [3] Patent: US2015/18367, 2015, A1. Location in patent: Paragraph 0173; 0174 [4] Patent: EP2570125, 2013, A1. Location in patent: Paragraph 0151 [5] Patent: WO2013/37960, 2013, A1. Location in patent: Page/Page column 74 [6] Patent: WO2013/26914, 2013, A1. Location in patent: Page/Page column 135 [7] Patent: WO2013/78468, 2013, A1. Location in patent: Paragraph 0526; 0527