Preparation of 2,3,5-trimethyl-p-benzoquinone
    4.
    发明授权
    Preparation of 2,3,5-trimethyl-p-benzoquinone 失效
    制备2,3,5-三甲基 - 对苯醌

    公开(公告)号:US5041572A

    公开(公告)日:1991-08-20

    申请号:US493103

    申请日:1990-03-13

    CPC分类号: C07C46/08

    摘要: 2,3,5-Trimethyl-p-benzoquinone is prepared by oxidation of trimethylphenol with oxygen or an oxygen-containing gas in the presence of a catalyst containing a copper(II) halide in a two-phase reaction medium consisting of water and an aliphatic alcohol at elevated temperatures by a process in which the reaction is carried out in a mixture of water and a saturated aliphatic alcohol of 12 to 18 carbon atoms, having a flashpoint greater than 120.degree. C., such as 1-dodecanol, 1-tetradecanol, 1-hexadecanol or 1-octadecanol, in particular 1-dodecanol, and at from 60.degree. to 100.degree. C.Particularly good yields of TMQ are obtained if the reaction is carried out in the presence of a copper(II) halide, such as CuCl.sub.2 or CuBr.sub.2, and of an alkaline earth metal halide, in particular CaCl.sub.2 or MgCl.sub.2, or of an alkali metal halide, in particular LiCl or NaCl, as the catalyst system.

    摘要翻译: 通过在含有卤化铜(II)的催化剂存在下,用氧或含氧气体氧化三甲基苯酚,制备2,3,5-三甲基对苯醌,所述两相反应介质由水和 脂族醇在高温下通过反应在水和12至18个碳原子的饱和脂族醇的混合物中进行的方法进行,其闪点大于120℃,如1-十二醇,1- 十四烷醇,1-十六烷醇或1-十八烷醇,特别是1-十二烷醇,以及60-100℃。如果反应在卤化铜(II)存在下进行,则得到特别好的收率的TMQ, 例如CuCl 2或CuBr 2,以及碱土金属卤化物,特别是CaCl 2或MgCl 2,或碱金属卤化物,特别是LiCl或NaCl,作为催化剂体系。

    Treatment of methanolic-aqueous residues from syntheses employing
triphenylphosphonium salts
    5.
    发明授权
    Treatment of methanolic-aqueous residues from syntheses employing triphenylphosphonium salts 失效
    使用三苯基鏻盐从合成处理甲醇 - 水残余物

    公开(公告)号:US4206153A

    公开(公告)日:1980-06-03

    申请号:US969665

    申请日:1978-12-15

    摘要: A process for treating residues which result from the Wittig synthesis of olefins and which consist principally of methanol, triphenylphosphine oxide, salts and organic by-products, by steam-stripping the volatile constituents, with partial condensation of the steam, and separating the resulting aqueous-organic mixture at 80.degree.-100.degree. C. into a saline aqueous phase and an organic phase containing principally triphenylphosphine oxide. Using this process provides a simple method of freeing, from triphenylphosphine oxide and other organic impurities, the effluent from syntheses which result in the formation of triphenylphosphine oxide, and thereby on the one hand substantially facilitates the purification of the effluent and on the other hand provides a simple method of recovering the triphenylphosphine oxide. The latter compound, which is easily purified by distillation or recrystallization, can then be used, for example, to prepare the triphenylphosphine required for Wittig syntheses or to prepare the triphenylphosphine dichloride required for the synthesis of pesticides.

    摘要翻译: 用于处理由Wittig合成烯烃产生的残余物的方法,其主要由甲醇,三苯基氧化膦,盐和有机副产物组成,通过汽提汽提挥发性成分,蒸汽部分冷凝,并将所得水溶液 - 有机混合物在80°-100℃下进入盐水水相和主要含有三苯基氧化膦的有机相。 使用该方法提供了从三苯基氧化膦和其它有机杂质释放导致形成三苯基氧化膦的合成流出物的简单方法,从而一方面大大有利于流出物的纯化,另一方面提供 回收三苯基氧化膦的简单方法。 然后可以通过蒸馏或重结晶容易地纯化的后者化合物,例如,制备Wittig合成所需的三苯基膦或制备合成农药所需的三苯基膦二氯化物。

    Production of dry powders of substances which are sensitive to oxidation
    7.
    发明授权
    Production of dry powders of substances which are sensitive to oxidation 失效
    生产对氧化敏感的物质的干粉

    公开(公告)号:US4519961A

    公开(公告)日:1985-05-28

    申请号:US413085

    申请日:1982-08-30

    摘要: A process for pulverizing substances which are sensitive to oxidation, in particular oily substances, by dispersing oil-soluble substances, e.g. vitamins, carotinoids, pharmaceutically active compounds or aromas, in an aqueous solution of a film-forming colloid, which constitutes the continuous phase of the dispersion, with the addition of one or more substances from the group comprising the mono-, di- and polysaccharides, atomizing the dispersion, in a spray tower, in the presence of a spraying assistant and collecting the resulting particles in a fluidized bed, wherein, as the spraying auxiliary, a hydrophobic silica or a metal salt of a higher fatty acid is introduced above the fluidized bed and distributed uniformly in the spraying space, at a temperature at which the colloid of the atomized particles has not yet solidified, and the assistant-laden particles, colloid material of which essentially has not yet gelatinized, is collected in a fluidized bed, and dried therein in a conventional manner.

    摘要翻译: 通过分散油溶性物质,例如粉碎对氧化敏感的物质,特别是油性物质的方法。 维生素,类胡萝卜素,药物活性化合物或香气,在构成分散体的连续相的成膜胶体的水溶液中,加入一种或多种包含单糖,二糖和多糖的物质 ,在喷雾塔中,在喷雾助剂的存在下雾化分散体,并将所得颗粒收集在流化床中,其中,作为喷雾助剂,将疏水性二氧化硅或高级脂肪酸的金属盐引入到 流化床,并且在雾化颗粒的胶体尚未固化的温度下均匀地分布在喷雾空间中,并且其主要尚未凝胶化的助粘剂颗粒(其胶体材料基本上尚未凝胶化)被收集在流化床中, 并以常规方式在其中干燥。

    Manufacture of tocopherol
    8.
    发明授权
    Manufacture of tocopherol 失效
    生育酚生产

    公开(公告)号:US4191692A

    公开(公告)日:1980-03-04

    申请号:US896479

    申请日:1978-04-14

    IPC分类号: C07D311/72

    CPC分类号: C07D311/72

    摘要: In the manufacture of tocopherol (vitamin E) by reaction of isophytol with trimethylhydroquinone in the presence of zinc chloride and acid in a hydrocarbon solvent one of the starting compounds, isophytol, is pretreated with small amounts of ammonia or an amine.Tocopherol is obtained in higher yield and purity.

    摘要翻译: 在氯化锌和酸在烃溶剂存在下,通过异山梨醇与三甲基对苯二酚的反应制造生育酚(维生素E),其中一种起始化合物异山梨醇,用少量的氨或胺进行预处理。 以更高的产率和纯度获得生育酚。