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    • 10. 发明授权
    • Process for separating mixtures of 3- and 4-nitrophthalic acid
    • 分离3-和4-硝基邻苯二甲酸的混合物的方法
    • US4284797A
    • 1981-08-18
    • US44122
    • 1979-05-31
    • Peter FurrerHarry Beyeler
    • Peter FurrerHarry Beyeler
    • C07C67/00C07C201/00C07C201/16C07C205/57C07C79/46
    • C07C201/16
    • A novel improved process for separating mixtures of 3- and 4-nitrophthalic acid is described. The said process comprises treating a mixture of 3- and 4-nitrophthalic acid, which mixture is free from inorganic acid residues, in an aqueous-organic medium containing 1-20 percent by volume of water, at a temperature of between 20.degree. and 100.degree. C., stepwise with a base capable of forming salts of 3- and 4-nitrophthalic acid, which salts are essentially insoluble in the reaction medium, the treatment being carried out by adding base until a pH value of about 2.8 is obtained, separating the precipitating product consisting mainly of a 3-nitrophthalic acid mono-salt, subsequently precipitating, by the addition of further base, a product consisting principally of a 4-nitrophthalic acid salt, and finally converting the resulting nitrophthalic acid salts separately into the corresponding free acids, and optionally purifying these. The 3- and 4-nitrophthalic acid can be obtained by the process according to the invention in a simple manner in an isomer-free form and in good to very good yields.
    • 描述了一种用于分离3-和4-硝基邻苯二甲酸的混合物的改进方法。 所述方法包括在含有1-20体积%水的含水有机介质中,在20至100℃的温度下处理3-和4-硝基邻苯二甲酸的混合物,该混合物不含无机酸残基 ℃,与能够形成3-和4-硝基邻苯二甲酸盐的碱分步,该盐基本上不溶于反应介质,该处理通过加入碱进行直到获得约2.8的pH值,分离 主要由3-硝基邻苯二甲酸单盐组成的沉淀产物,随后通过加入另外的碱沉淀出主要由4-硝基邻苯二甲酸盐组成的产物,最后将所得的硝基邻苯二甲酸盐分别转化为相应的无 酸,并任选地纯化这些。 3-和4-硝基邻苯二甲酸可以通过本发明的方法以简单的方式以无异构体的形式和良好至非常好的产率获得。