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    Preparation of 1-alkyl-2-chloro-5-nitrobenzene-4-sulfonic acids
    7.
    发明授权
    Preparation of 1-alkyl-2-chloro-5-nitrobenzene-4-sulfonic acids 失效
    1-烷基-2-氯-5-硝基苯-4-磺酸的制备

    公开(公告)号：US4427600A

    公开(公告)日：1984-01-24

    申请号：US343933

    申请日：1982-01-29

    申请人： Peter Tonne ,  Elisabeth R. Mueller ,  Helmut Goerth

    发明人： Peter Tonne ,  Elisabeth R. Mueller ,  Helmut Goerth

    IPC分类号： C07C309/40 ,  C07C67/00 ,  C07C301/00 ,  C07C303/06 ,  C07C303/22 ,  C07C143/24

    CPC分类号： C07C309/00

    摘要： A process for the preparation of compounds of the formula I ##STR1## where R is alkyl, by sulfonation, chlorination and nitration starting from an alkylbenzene, wherein the alkylbenzene is sulfonated with from 2.5 to 3, preferably from 2.65 to 2.75, moles of concentrated sulfuric acid per mole of alkylbenzene, the reaction product is then reacted with from about 1.1 to 1.3 moles of chlorine in the absence of a catalyst, the product is subsequently nitrated with highly concentrated nitric acid at elevated temperatures and the nitro compound is isolated.

    摘要翻译： 制备式I化合物的方法，其中R是烷基，通过从烷基苯开始的磺化，氯化和硝化，其中烷基苯用2.5至3，优选2.65至2.75摩尔的 浓硫酸/摩尔烷基苯，然后在不存在催化剂的情况下使反应产物与约1.1至1.3摩尔的氯反应，随后将产物在高温下用高度浓缩的硝酸进行硝化，并分离硝基化合物。

    Process for producing the magnesium salt of 3-nitro-naphthalene-1,5-disulfonic acid (nitro-Armstrong's acid)
    8.
    发明授权
    Process for producing the magnesium salt of 3-nitro-naphthalene-1,5-disulfonic acid (nitro-Armstrong's acid) 失效
    制备3-硝基 - 萘-1,5-二磺酸镁盐（硝基 - 阿姆斯壮酸）的方法

    公开(公告)号：US4348334A

    公开(公告)日：1982-09-07

    申请号：US113412

    申请日：1980-01-18

    申请人： Bernhard Albrecht ,  Hans Frey ,  Vinzenz Habermacher ,  Horst Behre ,  Lutz Kienitz ,  Wolfgang Schenk ,  Guido Steffan ,  Axel Vogel

    发明人： Bernhard Albrecht ,  Hans Frey ,  Vinzenz Habermacher ,  Horst Behre ,  Lutz Kienitz ,  Wolfgang Schenk ,  Guido Steffan ,  Axel Vogel

    IPC分类号： C07C309/40 ,  C07C67/00 ,  C07C301/00 ,  C07C303/06 ,  C07C303/22 ,  C07C303/32 ,  C07C143/55

    CPC分类号： C07C309/00

    摘要： A process for producing the magnesium salt of 3-nitro-naphthalene-1,5-disulfonic acid by sulfonating naphthalene, nitrating the sulfonation product, and separating the pure magnesium salt of 3-nitronaphthalene-1,5-disulfonic acid, which process comprises:(a) sulfonating naphthalene with liquid SO.sub.3 in the presence of an inert organic solvent at temperatures between -40.degree. and +20.degree. C.;(b) adding to the reaction mixture obtained a mixture consisting of about equal parts of 100% sulfuric acid and fully reacted crude nitration mixture from nitration of a previous nitration charge, separating from the resulting two-phase system the upper organic solvent phase by decanting, and removing from the Armstrong's acid anhydride acid slurry the remainder of organic solvent by distillation, or removing it during or after subsequent nitration, subsequently adding to the residue the amount of nitric acid required for nitration, and then nitrating;(c) adding then firstly water and afterwards, in the absence of the inert organic solvent, at 90.degree. to 120.degree. C., a compound releasing magnesium ions, the amount being such that, per mol of 3-nitronaphthalene-1,5-disulfonic acid, 1.1 to 1.3 mols of magnesium ions are added, and a sulfuric acid concentration of between 40 and 60 percent by weight (relative to the sulfuric acid and water) is maintained; and(d) separating the crystallized magnesium salt of 3-nitronaphthalene-1,5-disulfonic acid at a temperature of between 20.degree. and 70.degree. C., and subsequently optionally washing it with a maximum of 60 percent by weight of sulfuric acid and/or water, and optionally drying the product.

    摘要翻译： 通过磺化萘，硝化磺化产物和分离3-硝基萘-1,5-二磺酸的纯镁盐来生产3-硝基 - 萘-1,5-二磺酸的镁盐的方法，该方法包括 ：（a）在-40℃〜+ 20℃的温度下，在惰性有机溶剂的存在下，用液态SO 3磺化萘。 （b）向反应混合物中加入由约等量的100％硫酸组成的混合物和来自先前硝化装置的硝化的完全反应的粗硝化混合物，通过倾析从所得两相体系中分离出上部有机溶剂相 ，并通过蒸馏从阿姆斯壮的酸酐酸浆中除去剩余的有机溶剂，或者在后续硝化过程中或之后将其除去，随后向残余物中加入硝化所需的硝酸量，然后硝化; （c）然后首先加入水，然后在不存在惰性有机溶剂的情况下，在90〜120℃下，加入释放镁离子的化合物，其用量为每摩尔3-硝基萘-1,5 二磺酸，加入1.1〜1.3摩尔的镁离子，硫酸浓度保持在40〜60重量％之间（相对于硫酸和水）; 和（d）在20℃至70℃的温度下分离3-硝基萘-1,5-二磺酸的结晶镁盐，随后任选地用最多60重量％的硫酸洗涤， /或水，并任选地干燥产品。