化学合成。
化学合成
合成路线 1(1. 合成:14719-83-6)
产率:92%
合成条件:at 0℃; for 6 h; Heating / reflux
实验步骤:4-氯-3-硝基苯甲酸甲酯(1)。 将4-氯-3-硝基 - 苯甲酸(5.0g,24.8mmol)溶于200ml甲醇中,加入4.15ml(29.8mmol)三乙胺。 在冰盐浴中冷却,一滴一滴地加入3.19ml(44.7mmol)乙酰氯。 在回流下搅拌6小时。 减压蒸发溶剂。 用100ml水吸收残余物,用乙酸乙酯(100ml)萃取2次。 将有机相用MgSO 4干燥并在减压下蒸发,并用乙醚(10ml)(4.81g,92%)纯化。 Rf = 0.55(EtOAc /环己烷= 7/3); 熔点79-80℃。 ir CO 1716 cm-1; 1H-NMR(300MHz,DMSO-d6)δ3.90(s,3H,OCH3),7.90(d,1H,H5,J5-6 = 8.1Hz),8.15(dd,1H,H6,J6-5 = 8.1) Hz,J5-2 = 1.5Hz),8.49(d,1H,H2,J2-6 = 1.5Hz)。。(C8H6ClNO4)。
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