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    • 30. 发明授权
    • Method of making high purity substituted diphenyldisulfides
    • 制备高纯度取代二苯基二硫化物的方法
    • US5998670A
    • 1999-12-07
    • US40612
    • 1998-03-18
    • David Y. TangMichael C. HausladenViktor D. Sorokin
    • David Y. TangMichael C. HausladenViktor D. Sorokin
    • C07C319/24C07C321/30C07C323/09C07C321/00
    • C07C319/24
    • Disclosed is a method of making a substituted diphenyldisulfide from a substituted thiophenol. A two phase reaction mixture is prepared which comprises a substituted thiophenol having the general formula ##STR1## hydrogen peroxide, water, an organic solvent, a basic salt that will give a pH between about 7 and about 10, and an optional flocculating agent. In the formula, R is selected from the group consisting of halogen, alkyl from C.sub.1 to C.sub.6, alkoxy from C.sub.1 to C.sub.6, or nitro. After the exothermic reaction is complete, the reaction mixture is cooled to crystallize the substituted diphenyldisulfide product. The symmetrical product precipitates preferentially over the unsymmetrical product, thereby enhancing the purity of the product over the purity of the starting material. Optionally, the organic solvent and the aqueous phase are recycled.
    • 公开了从取代的苯硫酚制备取代的二苯基二硫化物的方法。 制备两相反应混合物,其包含具有通式过氧化氢,水,有机溶剂,将产生约7至约10的pH的碱性盐和任选的絮凝剂的取代的苯硫酚。 在该式中,R选自卤素,C1至C6的烷基,C1至C6的烷氧基或硝基。 放热反应完成后,冷却反应混合物以结晶取代的二苯基二硫化物产物。 对称产物优先于非对称产物沉淀,从而提高产品的纯度高于起始原料的纯度。 任选地,有机溶剂和水相再循环。