Synthesis of substituted mercapto-benzaldehydes
    1.
    发明授权
    Synthesis of substituted mercapto-benzaldehydes 有权
    取代的巯基 - 苯甲醛的合成

    公开(公告)号:US6025526A

    公开(公告)日:2000-02-15

    申请号:US248053

    申请日:1999-02-10

    CPC分类号: C07C319/14

    摘要: Disclosed is a composition of (1) a substituted benzaldehyde having the general formula ##STR1## where X is a leaving group in the ortho or para position, (2) a mercaptide having the general formula MSR' in an amount about stoichiometric to about 20 mole % in excess of stoichiometric with the amount of said substituted benzaldehyde, where M is an alkali metal and R' is alkyl or haloalkyl from C.sub.1 to C.sub.8 or aryl, aralkyl, or alkyl from C.sub.6 to C.sub.12, (3) sufficient water to dissolve said mercaptide and MX, (4) about 0.1 to about 5 mole %, based on said substituted benzaldehyde, of a phase transfer catalyst, and (5) 0 to about 100 wt %, based on total composition weight, of a water-immiscible organic solvent. Heating the composition to a temperature between about room temperature and 100.degree. C. results in the formation of a substituted mercapto-benzaldehyde.

    摘要翻译: 公开了(1)具有通式的取代的苯甲醛的组合物,其中X是邻位或对位的离去基团,(2)具有通式MSR'的硫醇,其量为约化学计量约20摩尔% 过量的化学计量与所述取代的苯甲醛的量,其中M是碱金属,R'是C1至C8的烷基或卤代烷基或芳基,芳烷基或C6至C12的烷基,(3)足够的水以溶解所述硫醇和 MX,(4)约0.1至约5摩尔%,基于所述取代的苯甲醛,相转移催化剂,和(5)0至约100重量%,基于总组合重量,与水不混溶的有机溶剂。 将组合物加热至约室温至100℃的温度,导致形成取代的巯基 - 苯甲醛。

    Method of making high purity substituted diphenyldisulfides
    2.
    发明授权
    Method of making high purity substituted diphenyldisulfides 失效
    制备高纯度取代二苯基二硫化物的方法

    公开(公告)号:US5998670A

    公开(公告)日:1999-12-07

    申请号:US40612

    申请日:1998-03-18

    CPC分类号: C07C319/24

    摘要: 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.

    摘要翻译: 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。