化学合成。
化学合成
合成路线 1(2. 合成:63897-12-1)
产率:85.7%
合成条件:at 95℃; for 1.50 h;
实验步骤:(1)将2,4-二氯-6-甲基-3-硝基吡啶-6-甲基-3-硝基吡啶-2,4-二醇(1.7g,10mmol)溶解于10mL POCl 3中,加热至95℃, 搅拌1.5小时。通过离心除去过量的POCl 3。 小心加入100mL冰水。反应溶液用乙酸乙酯(80mL×3)萃取。合并有机相,用饱和盐水洗涤,用无水Na 2 SO 4干燥,旋转干燥,得到1.773g黄色粉末。 产量为85.7%。
参考文献:
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