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    Preparation of 2,3,5-trimethyl-p-benzoquinone
    1.
    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

    申请人： Ulrich Hoercher ,  Barbara Jessel ,  Bernhard Bockstiegel ,  Paul Grafen ,  Harald Laas

    发明人： Ulrich Hoercher ,  Barbara Jessel ,  Bernhard Bockstiegel ,  Paul Grafen ,  Harald Laas

    IPC分类号： B01J27/122 ,  C07B61/00 ,  C07C46/08 ,  C07C50/02

    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。

    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 C10-C30-alkenes by partial hydrogenation of alkynes over fixed-bed supported palladium catalysts
    8.
    发明授权
    Preparation of C10-C30-alkenes by partial hydrogenation of alkynes over fixed-bed supported palladium catalysts 失效
    通过固定床负载的钯催化剂上的炔进行部分氢化制备C10-C30-烯烃

    公开(公告)号：US06365790B2

    公开(公告)日：2002-04-02

    申请号：US09734024

    申请日：2000-12-12

    申请人： Klaus Reimer ,  Gerd Kaibel ,  Ulrich Kammel ,  Franz Josef Bröcker ,  Andreas Ansmann ,  Heinz Etzrodt ,  Manfred Stroezel ,  Mathias Haake ,  Lothar Laupichler ,  Bernhard Bockstiegel

    发明人： Klaus Reimer ,  Gerd Kaibel ,  Ulrich Kammel ,  Franz Josef Bröcker ,  Andreas Ansmann ,  Heinz Etzrodt ,  Manfred Stroezel ,  Mathias Haake ,  Lothar Laupichler ,  Bernhard Bockstiegel

    IPC分类号： C07C2900

    CPC分类号： C07C29/17 ,  B01J23/44 ,  B01J23/50 ,  B01J35/04 ,  B01J35/06 ,  B01J37/0217 ,  B01J37/0225 ,  B01J37/08 ,  C07C5/09 ,  C07C2523/44 ,  C07C11/02 ,  C07C33/025 ,  C07C33/02

    摘要： Alkenes are prepared by partial hydrogenation of alkynes in the liquid phase at from 20 to 250° C. and hydrogen partial pressures of from 0.3 to 200 bar over fixed-bed supported palladium catalysts which are obtainable by heating the support material in the air, cooling, applying a palladium compound and, if required, additionally other metal ions for doping purposes, molding and processing to give monolithic catalyst elements, by a process in which A) alkynes of 10 to 30 carbon atoms are used as starting compounds, B) the palladium compound and, if required, the other metal ions are applied to the support material by impregnation of the heated and cooled support material with a solution containing palladium salts and, if required, other metal ions and subsequent drying, and C) from 10 to 2000 ppm of carbon monoxide (CO) are added to the hydrogenation gas or a corresponding amount of CO is allowed to form in the liquid phase by slight decomposition of a compound which is added to the reaction mixture and eliminates CO under the reaction conditions. The process is particularly advantageous if the partial hydrogenation is carried out in a tube reactor by the trickle-bed or liquid phase procedure with product recycling at cross-sectional loadings of from 20 to 500 m3/m2*h. The process is particularly suitable for the preparation of 3,7,11,15-tetramethyl-1-hexadecen-3-ol (isophytol), 3,7,11-trimethyl-l-dodecen-3-ol (tetrahydronerolidol), 3,7,11-trimethyl-1,4-dodecadien-3-ol, 3,7,11-trimethyl-1,6-dodecadien-3-ol (dihydronerolidol), 3,7-dimethyloct-1,6-dien-3-ol or 3,7-dimethyloct-1-en-3-ol from the corresponding alkynes.

    摘要翻译： 烯烃通过液相中炔烃在20至250℃的部分氢化和固定床负载的钯催化剂的0.3至200巴的氢分压来制备，其可通过加热空气中的载体材料，冷却 使用钯化合物，另外还需要另外的金属离子用于掺杂目的，通过使用10-30个碳原子的炔烃作为起始化合物的方法，模塑和加工以得到整体式催化剂元素，B）钯 如果需要，另外的金属离子通过用含有钯盐的溶液浸渍加热和冷却的载体材料以及如果需要的话其它金属离子并随后干燥而被施加到载体材料上，C）为10-2000ppm 的一氧化碳（CO）加入到氢化气体中，或者相应量的CO在液相中形成，通过轻微分解添加到真空中的化合物 并且在反应条件下消除CO。如果部分氢化在管式反应器中通过滴流床或液相方法进行，则该方法是特别有利的，其中产物回收的横截面负荷为20-500m 3 / m2 * h。 该方法特别适用于制备3,7,11,15-四甲基-1-十六碳烯-3-醇（异山梨糖醇），3,7,11-三甲基-1-十二碳烯-3-醇（四氢化吗啉醇），3 ，7,11-三甲基-1,4-十二碳二烯-3-醇，3,7,11-三甲基-1,6-十二碳二烯-3-醇（二氢吗啉醇），3,7-二甲基辛-1,6-二烯 - 3-醇或3,7-二甲基辛-1-烯-3-醇。

    Preparation of .gamma.,.delta.-unsaturated ketones by the Carroll reaction, novel catalysts therefor and the preparation thereof
    9.
    发明授权
    Preparation of .gamma.,.delta.-unsaturated ketones by the Carroll reaction, novel catalysts therefor and the preparation thereof 失效
    通过Carroll反应制备γ，δ-不饱和酮，其新型催化剂及其制备

    公开(公告)号：US6051741A

    公开(公告)日：2000-04-18

    申请号：US168378

    申请日：1998-10-08

    申请人： Heinz Etzrodt ,  Dietmar Weller ,  Carsten Oost ,  Hagen Jaedicke ,  Manfred Stroezel ,  Bernhard Bockstiegel ,  Lothar Laupichler ,  Klaus Reimer

    发明人： Heinz Etzrodt ,  Dietmar Weller ,  Carsten Oost ,  Hagen Jaedicke ,  Manfred Stroezel ,  Bernhard Bockstiegel ,  Lothar Laupichler ,  Klaus Reimer

    IPC分类号： B01J31/02 ,  B01J31/14 ,  C07B61/00 ,  C07C45/67 ,  C07C45/68 ,  C07C49/203 ,  C07F5/06 ,  C07C45/00

    CPC分类号： C07F5/069 ,  B01J31/0211 ,  C07C45/676

    摘要： A process for preparing .gamma.,.delta.-unsaturated ketones of the general formula I ##STR1## by reacting an allyl alcohol of the general formula II ##STR2## in which R.sup.1 is H or a hydrocarbon radical having 1 to 20 carbon atoms, with diketene or an alkyl acetoacetate of the general formula III ##STR3## in which R.sup.2 is alkyl having 1 to 4 carbon atoms in an unmodified or modified Carroll reaction in the presence of an aluminum catalyst, wherein aluminum compounds which are stable liquids at room temperature, or a mixture of such aluminum compounds, which comprise at least one radical formed from an alkyl acetoacetate and 1 or 2 alkoxy radicals, or else comprise exclusively radicals formed from alkyl acetoacetates, which are esterified with sec-butanol or isobutanol, or else are esterified with at least two different alcohols, are used as aluminum catalyst. Also claimed are the novel mixtures of aluminum compounds which comprise radicals which are formed exclusively from alkyl acetoacetates and are esterified with at least two different alkanols, and the batchwise and continuous preparation of the liquid aluminum catalysts.

    摘要翻译： 通过使通式II的烯丙醇（其中R 1为H或具有1至20个碳原子的烃基）的烯丙醇与二烯酮或一般的乙酰乙酸烷基酯反应制备通式I的γ，β-不饱和酮的方法 式III其中R2是在未改性或改性的Carroll反应中在铝催化剂存在下具有1至4个碳原子的烷基，其中在室温下为稳定液体的铝化合物或这种铝化合物的混合物，其包含在 由烷基乙酰乙酸酯和1或2个烷氧基形成的至少一个基团，或者仅由烷基乙酰乙酸酯形成的由仲丁醇或异丁醇酯化的酰基或者由至少两种不同的醇酯化的基团用作铝 催化剂。 还要求的是铝化合物的新型混合物，其包含仅由乙酰乙酸烷基酯形成并且与至少两种不同的链烷醇酯化的基团，以及液体铝催化剂的分批连续制备。