化学合成。
化学合成
合成路线 1(1. 合成:3843-97-8)
产率:100%
合成条件:With iron(III) chloride; amino aminoalcohol In methanol at 20 - 80℃; for 5 h; Sealed tube
实验步骤:步骤3:ο4-氯-1-乙基-2-硝基苯(0.9g,4.9mmol),氯化铁(III)(0.13g,0.49mmol)和木炭(80mg,6.6mmol)在甲醇中的混合物 向(17ml)中加入水合肼(0.95ml,20mmol)的甲醇(7ml)溶液。 在室温下搅拌反应混合物,同时放出气体。 当气体逸出停止时,将小瓶密封并在80℃下加热5小时(**压力随时间增加并且小瓶需要经常排出)。 将混合物冷却至室温并通过硅藻土过滤,用甲醇洗涤,浓缩,并通过硅胶色谱法(梯度0至50%EtOAc /己烷)纯化。 产物苯胺4是浅黄色油(定量); 1H NMR(400MHz,DMSO-d6)δ6.86(dd,= 8.0,0.7Hz,1H),6.59(d,= 2.2Hz,1H),6.44(dd,7 = 8.0,2.2Hz,1H),5.11 (s,2H),2.43-2.31(m,2H),1.06(t,J = 7.5Hz,3H)。
参考文献:
- [1] Patent: WO2016/106331, 2016, A1. Location in patent: Paragraph 0222 [2] Patent: WO2012/139930, 2012, A1. Location in patent: Page/Page column 72 [3] Patent: WO2012/143248, 2012, A1. Location in patent: Page/Page column 24 [4] Patent: WO2014/19908, 2014, A2. Location in patent: Page/Page column 33 [5] Patent: US2014/51708, 2014, A1. Location in patent: Paragraph 0722; 0723 [6] Journal of Organic Chemistry, 1957, vol. 22, p. 639,641 [7] Patent: US2012/15962, 2012, A1. Location in patent: Page/Page column 75 [8] Patent: CN104163764, 2016, B. Location in patent: Paragraph 0050-0053 [9] Patent: WO2017/223202, 2017, A1. Location in patent: Paragraph 0119