化学合成。
化学合成
合成路线 1(1. 合成:2770-11-8)
产率:78%
合成条件:Stage #1: With iron; ammonium chloride In ethanol; water for 1 h; Heating / reflux
实验步骤:2-(4-氯苯氧基)苯胺(AMR01029)C12H10ClNO,分子量219.67。先前描述:Wardrop,A.W。H .; 戈登,L。S。; 哈里森,J。M。; 英寸,T。D. J. Chem。 Soc,Perkin I1976,1276-1285可商购获得的铁粉(3.18g,57.28mmol)和氯化铵(383mg,7.15mmol)在乙醇(45mL)和水(8mL)中的回流混合物加入l-( 将2,4-二氯苯氧基)-2-硝基苯(AMR01028,2.2g,8.81mmol)和所得混合物在回流下搅拌1小时。 除去溶剂后,将残余物在碳酸氢钠水溶液(40mL)中稀释,并用DCM(3×20mL)萃取。 将有机层干燥(MgSO 4),过滤并蒸发,得到AMR01029(1.50g,78%),为无色油状物,将其不经进一步纯化用于下一步骤。 Rf:0.53(DCM)1H NMR(270MHz,CDCl3).3.77(2H,br s,NH2),6.71(1H,m),6.83(2H,m),6.89(2H5 AA'BB'), 6.99(IH,m)和7.25(2H,AA'BB')。
参考文献:
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