化学合成。
化学合成
合成路线 1(1. 合成:112970-44-2)
产率:100%
合成条件:With hydrogenchloride; iron In ethanol for 1.50 h; Reflux
实验步骤:步骤1.合成2-溴-3-甲氧基苯胺(C23)将铁(1.94g,34mmol)加入到2-溴-1-甲氧基-3-硝基苯(2.50g,10.77mmol)的乙醇溶液中( 加入18mL)和浓盐酸(1mL),将反应混合物加热回流1.5小时。将混合物冷却至室温,通过硅藻土过滤并真空浓缩,得到标题化合物,为固体。 产量:2.57g,10.77mmol,100%。 LCMS m / z 202.1(M + 1).1 H NMR(400MHz,CD3OD)δ3.77(s,3H),6.30(d,J = 8.0Hz,1H),6.43(d,J = 8.0Hz,1H) ,6.98(dd,J = 8.0,8.0Hz,1H)。
参考文献:
- [1] Patent: US2012/252758, 2012, A1. Location in patent: Page/Page column 27 [2] Journal of Medicinal Chemistry, 2015, vol. 58, # 23, p. 9287 - 9295 [3] Patent: US2007/78147, 2007, A1. Location in patent: Page/Page column 67 [4] Patent: WO2018/13774, 2018, A1. Location in patent: Page/Page column 318 [5] Patent: EP3239143, 2017, A2. Location in patent: Paragraph 0441 [6] Patent: WO2004/103996, 2004, A1. Location in patent: Page 40-41 [7] Patent: WO2006/7700, 2006, A1. Location in patent: Page/Page column 62 [8] Patent: US2006/19905, 2006, A1. Location in patent: Page/Page column 24-25 [9] Patent: WO2006/85, 2006, A1. Location in patent: Page/Page column 75-76 [10] Patent: WO2007/9227, 2007, A1. Location in patent: Page/Page column 35 [11] Patent: WO2007/14919, 2007, A1. Location in patent: Page/Page column 91 [12] Journal of Organic Chemistry, 1988, vol. 53, # 6, p. 1170 - 1176 [13] Synthetic Communications, 2007, vol. 37, # 16, p. 2777 - 2786 [14] Bulletin of the Chemical Society of Japan, 1978, vol. 51, p. 2437 - 2438 [15] Journal of Medicinal Chemistry, 2006, vol. 49, # 17, p. 5352 - 5362