化学合成。
化学合成
合成路线 1(1. 合成:163733-99-1)
产率:92%
合成条件:With hydrogen In methanol for 2 h;
实验步骤:将1-苄氧基-2,3-二氟-4-硝基苯(14g,52.8mmol)和Pd / C(10%,1.4g)在MeOH(200mL)中的混合物在氢气氛(30psi)下搅拌。 2小时 过滤除去催化剂,滤液真空浓缩,得到4-氨基-2,3-二氟 - 苯酚(7g,收率92%)。 1H NMR(400MHz,DMSO-d6)δ9.05(s,1H),6.45(t,J = 8.8Hz,1H),6.34(t,J = 9.2Hz,1H),4.67(s,2H)。
参考文献:
- [1] Patent: US2008/90856, 2008, A1. Location in patent: Page/Page column 41 [2] Patent: WO2010/51373, 2010, A1. Location in patent: Page/Page column 61 [3] Patent: WO2013/36232, 2013, A2. Location in patent: Paragraph 00279 [4] Patent: WO2013/180949, 2013, A1. Location in patent: Paragraph 0180 [5] Patent: WO2014/22116, 2014, A2. Location in patent: Paragraph 0177 [6] Patent: US2015/37280, 2015, A1. Location in patent: Paragraph 0303-0305