化学合成。
化学合成
合成路线 1(1. 合成:101623-69-2)
产率:97%
合成条件:With pyridine In dichloromethane at 0 - 20℃; for 1.50 h;
实验步骤:向含有对硝基苯酚(1.39g,10mmol)和吡啶(0.81g,10mmol)的二氯甲烷(60mL)的冰冷反应混合物中加入氯甲酸1-氯乙酯(1.2mL,11mmol)。 将混合物在0℃下搅拌30分钟,然后在室温下搅拌1小时。 减压除去溶剂后,将残余物溶于乙醚中,用水,10%柠檬酸和水洗涤。 乙醚层用Na 2 SO 4干燥,减压蒸发,得到2.4g(97%)标题化合物(57),为灰白色固体。 1H NMR(CDCl3):1.93(d,3H),6.55(q,1H),7.42(d,2H),8.28(d,2H)。
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