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    Preparation of substituted phenols
    2.
    发明授权
    Preparation of substituted phenols 失效
    取代苯酚的制备

    公开(公告)号：US4538009A

    公开(公告)日：1985-08-27

    申请号：US599574

    申请日：1984-04-12

    申请人： Norbert Goetz ,  Harald Laas ,  Peter Tavs ,  Leopold Hupfer ,  Karl Baer

    发明人： Norbert Goetz ,  Harald Laas ,  Peter Tavs ,  Leopold Hupfer ,  Karl Baer

    IPC分类号： C07C37/055 ,  B01J23/00 ,  B01J23/42 ,  B01J23/44 ,  B01J23/58 ,  B01J23/60 ,  B01J23/89 ,  C07B61/00 ,  C07C27/00 ,  C07C37/06 ,  C07C37/07 ,  C07C39/06 ,  C07C67/00

    CPC分类号： C07C37/07 ,  B01J23/005 ,  B01J23/58 ,  B01J23/60 ,  B01J23/89 ,  C07C37/06

    摘要： Substituted phenols of the general formula I ##STR1## where R.sup.1, R.sup.2, R.sup.3, R.sup.4 and R.sup.5 are each hydrogen or an aliphatic or aromatic hydrocarbon radical, are prepared by dehydrogenating a cyclic alcohol of the general formula II ##STR2## or a cyclic ketone of the general formula III ##STR3## where one of the broken lines can be an additional C-C bond, in the gas phase at from 150.degree. to 380.degree. C. over a supported noble metal catalyst, by a process in which the dehydrogenation catalyst used is palladium or platinum on an aluminum spinel carrier, in particular an aluminum spinel which has a BET specific surface area of from 5 to 150 m.sup.2 /g or, for the dehydrogenation of cyclohexenones, preferably from 10 to 50 m.sup.2 /g. Particularly suitable aluminum spinels are those which, in addition to aluminum, contain magnesium, zinc, cobalt or nickel.In the novel process, substituted phenols are obtained in high yields and selectivities, and the catalyst has an extremely long life without a significant decrease in activity.

    摘要翻译： 通式Ⅰ的取代的酚Ⅰ，其中R 1，R 2，R 3，R 4和R 5各自为氢或脂族或芳族烃基，通过将通式II II的环醇脱氢或 环状酮，其中一条虚线可以是额外的CC键，在负载型贵金属催化剂的150〜380℃的气相中，其中， 所用的脱氢催化剂是钯尖晶石载体上的钯或铂，特别是BET比表面积为5〜150m 2 / g的尖晶石，或者环己烯酮的脱氢优选为10〜50m2 / g。 特别合适的铝尖晶石是除了铝之外还含有镁，锌，钴或镍的铝尖晶石。 在新方法中，以高产率和选择性获得取代的酚，并且催化剂具有极长的寿命而没有显着降低活性。

    Process for the preparation of a bis-salicylidene-alkylene-diaminocobaltous ion complex
    3.
    发明授权
    Process for the preparation of a bis-salicylidene-alkylene-diaminocobaltous ion complex 失效
    制备双亚水杨基 - 亚烷基 - 二氨基钴胺离子络合物的方法

    公开(公告)号：US4562277A

    公开(公告)日：1985-12-31

    申请号：US571806

    申请日：1984-01-18

    申请人： Harald Laas ,  Peter Tavs ,  Heinz Hannebaum ,  Manfred Stroezel

    发明人： Harald Laas ,  Peter Tavs ,  Heinz Hannebaum ,  Manfred Stroezel

    IPC分类号： C07C46/08 ,  C07F15/06

    CPC分类号： C07F15/065 ,  C07C46/08

    摘要： Improved process for the preparation of salcomine useful as an oxidation catalyst for the oxidation of alkylated phenols to the corresponding alkylated p-benzoquinones by reacting salicylaldehyde with ethylenediamine in a mole ratio of about 2:1 and a cobalt salt in a liquid reaction medium wherein the reaction medium is a linear or cyclic carboxamide which is disubstituted on the nitrogen, in particular dimethylformamide, and the cobalt salt is cobalt carbonate or with the cobalt hyroxide carbonate, 2 CoCO.sub.3.3 Co(OH).sub.2.H.sub.2 O. Preparation of the salcomine in accordance with the invention offers significant advantages, both in the preparation of the salcomine itself and in the subsequent oxidation of the trimethylphenol to trimethyl-p-benzoquinone utilizing the salcomine.

    摘要翻译： 通过使水杨醛与乙二胺以约2:1的摩尔比和在液体反应介质中的钴盐反应，将烷基化酚氧化成相应的烷基化对苯醌的氧化催化剂改进的改进方法，其中 反应介质是在氮气上二取代的直链或环状的酰胺，特别是二甲基甲酰胺，钴盐是碳酸钴或与钴酸钴2 CoCO 3·3 Co（OH）2·H 2 O. 根据本发明的沙门氏菌素的制备在使用沙门氏菌的情况下，在制备沙门酸本身和随后的三甲基苯酚氧化成三甲基对苯醌时具有显着的优点。

    Increasing the yield of 2.5.6-trimethylcyclohex-2-en-1-one
    4.
    发明授权
    Increasing the yield of 2.5.6-trimethylcyclohex-2-en-1-one 失效
    提高2.5.6-三甲基环己-2-烯-1-酮的产率

    公开(公告)号：US4820874A

    公开(公告)日：1989-04-11

    申请号：US111603

    申请日：1987-10-23

    申请人： Peter Tavs ,  Harald Laas ,  Horst Schauer ,  Lothar Arnold

    发明人： Peter Tavs ,  Harald Laas ,  Horst Schauer ,  Lothar Arnold

    IPC分类号： C07C45/74 ,  C07C45/78 ,  C07C45/82 ,  C07C45/85 ,  C07C49/603 ,  C07C45/67

    CPC分类号： C07C49/603 ,  C07C45/74 ,  C07C45/78 ,  C07C45/82 ,  C07C45/85

    摘要： The yield of 2,5,6-trimethyl-cyclohex-2-en-1-one is increased by reacting diethyl ketyone, in the presence of an alkali, with crotonaldehyde or a compound which is converted to crotonaldehyde under the reaction conditions chose, and working up the reaction mixture by distillation, by a method in which the distillation residue obtained is either(a) heated at from 120.degree. to 250.degree. C. in particular from 120.degree. to 200.degree. C., with the addition of a catalytic amount of an alkali, or(b) heated at from 150.degree. to 250.degree. C. without the addition of such a substance,and the mixture of 2,5,6-trimethylcyclohex-2-en-1-one and diethyl ketone which is formed from the distillation residue as a result of the heat treatment is separated by distillation.

    摘要翻译： 在碱存在下，使二乙基酮与巴豆醛或在选择的反应条件下转化为巴豆醛的化合物反应，使2,5,6-三甲基 - 环己-2-烯-1-酮的产率增加， 并通过蒸馏处理反应混合物，通过其中所得蒸馏残余物（a）在120℃至250℃，特别是120℃至200℃加热的方法，加入催化剂 碱的量，或（b）在不加入这种物质的情况下在150-250℃下加热，以及2,5,6-三甲基环己-2-烯-1-酮和二乙基酮的混合物，其中 由蒸馏残渣形成的热处理结果通过蒸馏分离。

    Preparation of .alpha.-tocopherol or .alpha.-tocopheryl acetate by reacting trimethylhydroquinone and phytol or isophytol, with recycling of the zinc halide condensation catalyst
    5.
    发明授权
    Preparation of .alpha.-tocopherol or .alpha.-tocopheryl acetate by reacting trimethylhydroquinone and phytol or isophytol, with recycling of the zinc halide condensation catalyst 失效
    通过三甲基对苯二酚和植物醇或异植醇反应制备α-生育酚或α-生育酚乙酸酯，再加上卤化锌缩合催化剂

    公开(公告)号：US6005122A

    公开(公告)日：1999-12-21

    申请号：US990092

    申请日：1997-12-12

    申请人： Kai-Uwe Baldenius ,  Wulf Kaiser ,  Bernhard Bockstiegel ,  Harald Laas ,  Bernhard Schulz ,  Peter Schmitt ,  Helmut Glietenberg

    发明人： Kai-Uwe Baldenius ,  Wulf Kaiser ,  Bernhard Bockstiegel ,  Harald Laas ,  Bernhard Schulz ,  Peter Schmitt ,  Helmut Glietenberg

    IPC分类号： B01J27/138 ,  C07D311/72

    CPC分类号： C07D311/72 ,  B01J27/138

    摘要： A process for preparing .alpha.-tocopherol or .alpha.-tocopheryl acetate by reacting 2,3,5-trimethylhydroquinone with isophytol or phytol in the presence of a zinc halide condensation catalyst and a proton donor in a solvent with or without subsequent esterification with acetic anhydride, which comprisesA. carrying out the reaction in a nonpolar solvent which is only slightly water-miscible, if at all andB. introducing the required zinc halide into the reaction in the form of a mixture of from 1 to 4 mol of water per mol of zinc halide.The possibility of introducing the zinc halide required in the process according to the invention in the form of a mixture of zinc halide and water which can be readily handled and metered at from 50 to 200.degree. C. without impairing the yield and purity of the tocopherol opens the way to an advantageous recycling of the zinc halide after the reaction by separating off or extracting and recycling the zinc halide in the form of a from 60 to 90% strength by weight solution or pumpable magma.

    摘要翻译： 在卤化锌缩合催化剂和质子供体存在下，使2,3,5-三甲基氢醌与异麦芽糖醇或植物醇在溶剂中反应制备α-生育酚或α-生育酚乙酸酯的方法，其中或不用随后用乙酸酐酯化， 其包括A.在非极性溶剂中进行反应，所述非极性溶剂仅仅是轻微的水混溶性的，如果有的话，则B.将所需的卤化锌以每摩尔1至4摩尔水的混合物的形式引入反应中 的卤化锌。 将本发明方法中所需的卤化锌以卤化锌和水的混合物的形式引入卤化物的可能性，其可以在50-200℃下容易地处理和计量，而不损害生育酚的产率和纯度 打开通过分离或提取和重新使用60至90％重量浓度的溶液或可泵送岩浆形式的卤化锌，从而在反应之后有效地再循环卤化锌。

    Preparation of tocopheral carboxylates or tocotrienyl esters by acid-catalyzed reaction with carboxylic acids
    8.
    发明授权
    Preparation of tocopheral carboxylates or tocotrienyl esters by acid-catalyzed reaction with carboxylic acids 失效
    通过与羧酸的酸催化反应制备生育酚羧酸酯或生育三烯基酯

    公开(公告)号：US06365758B1

    公开(公告)日：2002-04-02

    申请号：US09013813

    申请日：1998-01-26

    申请人： Joanna Linda von dem Bussche-Hünnefeld ,  Hagen Jaedicke ,  Guido Harms ,  Harald Laas

    发明人： Joanna Linda von dem Bussche-Hünnefeld ,  Hagen Jaedicke ,  Guido Harms ,  Harald Laas

    IPC分类号： C07D31104

    CPC分类号： C07D311/72

    摘要： A process for preparing tocopheryl esters or tocotrienyl esters by acid-catalyzed esterification of a tocopherol or a tocotrienol in a solvent while stirring at elevated temperature, which comprises a) carrying out the esterification with the appropriate carboxylic acid, b) carrying out the esterification with from 2.5 to 6 mol of the carboxylic acid in an aliphatic, cycloaliphatic or aromatic hydrocarbon boiling in the range from 80 to 200° C., or else with from 1.0 to 2.5 mol of the carboxylic acid in a mixture consisting of an aliphatic or cycloaliphatic hydrocarbon boiling in the range from 80 to 200° C. and a cyclic carbonate of the formula II or a &ggr;-lactone of the formula III  where R1, R2 and R3 are each H or lower alkyl, and R4 is H, lower alkyl, phenyl or methoxymethyl, as solvent, c) using a nonoxidizing strong inorganic or organic acid, preferably sulfuric acid, boroxalic acid or benzene- or toluenesulfonic acids, in catalytic amounts as acid catalyst, and d) continuously removing the water formed in the reaction by azeotropic distillation during the reaction.

    摘要翻译： 一种在高温下搅拌下在溶剂中通过酸催化酯化生育酚或生育三烯酚制备生育酚酯或生育三烯基酯的方法，该方法包括a）用合适的羧酸进行酯化，b）进行酯化反应 在80至200℃范围内沸腾的脂肪族，脂环族或芳族烃中的羧酸为2.5至6摩尔，或者由脂族或脂环族烃组成的混合物中的1.0至2.5摩尔羧酸 沸程在80至200℃的范围内，和式II的环状碳酸酯或式III的γ-内酯，其中R 1，R 2和R 3各自为H或低级烷基，且R 4为H，低级烷基，苯基 或甲氧基甲基，作为溶剂，c）使用非氧化的强无机或有机酸，优选硫酸，硼酸或苯或甲苯磺酸，催化量为酸催化剂，并且d）连续重新 在反应期间通过共沸蒸馏移动反应中形成的水​​。