1673-47-8 3-氯苯甲酰肼

危险性质：非危险化学品

化学合成。

化学合成

合成路线 1（1. 合成：1673-47-8）

产率：88% 合成条件：With hydrazine hydrate In ethanol; waterReflux 实验步骤：一般步骤：通过一锅常规方法合成酰肼（30-58）。将苯甲酸或其衍生物（10mmol）溶于乙醇（20mL）中。 加入硫酸（3N，2mL）并将反应内容物回流6小时。 用TLC监测反应。 反应完成后，通过加入固体NaHCO 3中和反应混合物，并过滤除去过量的NaHCO3。 在含有乙酯的中和反应混合物中，加入一水合肼（1.5mL，3mmol）并回流3-6小时以完成反应。通过蒸馏除去乙醇和未反应的肼至1/3体积。 将反应内容物冷却，过滤并用甲醇重结晶，得到所需的酰肼晶体（参见支持信息）。 参考文献：

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合成路线 2（3. 合成：1673-47-8）

产率：53% 合成条件：With dmap; hydrazine hydrate In methanol; ethanol; dichloromethane 实验步骤：3-氯苯甲酰肼将3-氯苯甲酸（0.5g，3.19mmol），1,3-二环己基碳二亚胺（0.72g，3.51mmol），4-二甲基氨基吡啶（0.04g，0.32mmol）在乙醇中的混合物在环境温度下搅拌1.5 小时。 滤出白色固体，滤液用二氯甲烷（100mL）稀释。 用1N硫酸氢钠（100mL），饱和碳酸氢钠（100mL），水（100mL）和盐水（100mL）洗涤有机溶液。 有机相用无水硫酸镁干燥并过滤。 将滤液真空浓缩。 将粗残余物溶于乙醇（15mL）中并用一水合肼（0.46mL，9.58mmol）处理。 将得到的澄清溶液在环境温度下搅拌过夜。 然后将反应混合物真空浓缩至干。 使用3％甲醇的二氯甲烷溶液对残余物进行硅胶色谱法，得到0.29g（53％）3-氯苯甲酰肼，为白色固体。 参考文献：

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