化学合成。
化学合成
合成路线 1(1. 合成:13575-75-2)
产率:93.3%
合成条件:With polyphosphoric acid In dichloromethane for 2 h; Reflux
实验步骤:将多磷酸(210g)加入到溶解在二氯甲烷(50mL)中的化合物4(0.19mol,42g)中,并将混合物在回流下加热2小时。 反应完成后,除去溶剂,将残余物缓慢加入碎冰中。 将溶液的pH值调节至7-8,过滤沉淀物并干燥,得到化合物5,为白色固体(36g,93.3%),Mp:94-96℃(点亮:96- 98°C [50])。 1 H NMR(400MHz,CDCl 3):δ7.51(s,1H),6.67(s,1H),3.93(s,3H),3.91(s,3H),2.89(t,J = 6Hz,2H), 2.60(t,J = 6.4Hz,2H),2.15-2.09(m,2H); 13 C NMR(101MHz,CDCl 3):δ197.10,153.51,147.96,139.27,125.79,110.22,108.57,55.98,38.50,29.44,23.61。
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