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1. 发明授权

US07547807B2 Method for producing phosphonium salts 有权
标题翻译：鏻盐的制备方法
公开(公告)号：US07547807B2
公开(公告)日：2009-06-16
申请号：US10582912
申请日：2004-12-14
申请人： Laszlo Szarvas , Klemens Massonne , Harald Laas , Kai Michael Exner , Detlev Glas
发明人： Laszlo Szarvas , Klemens Massonne , Harald Laas , Kai Michael Exner , Detlev Glas
IPC分类号： C07C315/00
CPC分类号： C07F9/5428 , C07F9/5442
摘要： The present invention relates to a process for preparing quaternary phosphonium salts by reacting a ternary phosphine with an optionally substituted, saturated or monounsaturated or polyunsaturated electrophile having from 3 to 25 carbon atoms in ternary solvent mixtures.
摘要翻译：本发明涉及通过使三元膦与在三元溶剂混合物中具有3至25个碳原子的任选取代的饱和或不饱和或多不饱和亲电体反应来制备季鏻盐的方法。

2. 发明申请

US20090043121A1 METHOD FOR PRODUCING VITAMIN A ACETATE 审中-公开
标题翻译：维生素A的制备方法
公开(公告)号：US20090043121A1
公开(公告)日：2009-02-12
申请号：US12255460
申请日：2008-10-21
申请人： Kai Michael Exner , Klemens Massonne , Harald Laas , Detlev Glas , Laszlo Szarvas
发明人： Kai Michael Exner , Klemens Massonne , Harald Laas , Detlev Glas , Laszlo Szarvas
IPC分类号： C07C69/612
CPC分类号： C07C403/12 , C07C2601/16
摘要： The present invention relates to a process for preparing vitamin A acetate by reacting β-vinylionol with triphenylphosphine in the presence of sulfuric acid in a solvent mixture consisting of 60 to 80% by weight methanol, 10 to 20% by weight water and 10 to 20% by weight aliphatic, cyclic or aromatic hydrocarbons having 5 to 8 carbon atoms to give β-ionylideneethyltriphenylphosphonium salts and subsequent Wittig reaction with 4-acetoxy-2-methylbut-2-enal.
摘要翻译：本发明涉及一种制备维生素A乙酸酯的方法，该方法是在硫酸存在下，使β-乙烯醇与三苯膦反应，在60至80％（重量）甲醇，10至20％（重量）水和10至20份重量％的具有5至8个碳原子的脂族，环状或芳族烃，得到β-离子亚乙基三苯基鏻盐，随后与4-乙酰氧基-2-甲基丁-2-烯的维t希反应。

3. 发明申请

US20070123726A1 Method for producing phosphonium salts 有权
标题翻译：鏻盐的制备方法
公开(公告)号：US20070123726A1
公开(公告)日：2007-05-31
申请号：US10582912
申请日：2004-12-14
申请人： Laszlo Szarvas , Klemens Massonne , Harald Laas , Kai Exner , Detlev Glas
发明人： Laszlo Szarvas , Klemens Massonne , Harald Laas , Kai Exner , Detlev Glas
IPC分类号： C07F9/02
CPC分类号： C07F9/5428 , C07F9/5442
摘要： The present invention relates to a process for preparing quaternary phosphonium salts by reacting a ternary phosphine with an optionally substituted, saturated or monounsaturated or polyunsaturated electrophile having from 3 to 25 carbon atoms in ternary solvent mixtures.
摘要翻译：本发明涉及通过使三元膦与在三元溶剂混合物中具有3至25个碳原子的任选取代的饱和或不饱和或多不饱和亲电体反应来制备季鏻盐的方法。

4. 发明申请

US20070082950A1 Method for producing vitamin a acetate 审中-公开
标题翻译：生产乙酸维生素的方法
公开(公告)号：US20070082950A1
公开(公告)日：2007-04-12
申请号：US10580958
申请日：2004-12-14
申请人： Kai Exner , Klemens Massonne , Harald Laas , Detlev Glas , Laszlo Szarvas
发明人： Kai Exner , Klemens Massonne , Harald Laas , Detlev Glas , Laszlo Szarvas
IPC分类号： C07C67/02 , A61K31/22
CPC分类号： C07C403/12 , C07C2601/16
摘要： The present invention relates to a process for preparing vitamin A acetate by reacting β-vinylionol with triphenylphosphine in the presence of sulfuric acid in a solvent mixture consisting of 60 to 80% by weight methanol, 10 to 20% by weight water and 10 to 20% by weight aliphatic, cyclic or aromatic hydrocarbons having 5 to 8 carbon atoms to give β-ionylideneethyltriphenylphosphonium salts and subsequent Wittig reaction with 4-acetoxy-2-methylbut-2-enal.
摘要翻译：本发明涉及一种制备维生素A乙酸酯的方法，该方法是在硫酸存在下，使β-乙烯醇与三苯膦反应，在60至80％（重量）甲醇，10至20％（重量）水和10至20份重量％的具有5至8个碳原子的脂族，环状或芳族烃，得到β-离子亚乙基三苯基鏻盐，随后与4-乙酰氧基-2-甲基丁-2-烯的维t希反应。

5. 发明授权

US4600799A Preparation of trimethylhydroquinone 失效
标题翻译：三甲基氢醌的制备
公开(公告)号：US4600799A
公开(公告)日：1986-07-15
申请号：US699194
申请日：1985-02-07
申请人： Franz J. Broecker , Peter Tavs , Harald Laas , Wolf-Karlo Aders
发明人： Franz J. Broecker , Peter Tavs , Harald Laas , Wolf-Karlo Aders
IPC分类号： C07C37/07
CPC分类号： C07C37/07
摘要： 2,3,6-Trimethylhydroquinone is prepared by catalytic hydrogenation of 2,3,6-trimethylquinone with hydrogen in the presence of a solvent by a continuous process in which the reaction is carried out over a platinum/alumina catalyst.
摘要翻译： 2,3,6-三甲基氢醌通过在溶剂存在下用氢气将2,3,6-三甲基醌催化氢化，其中反应在铂/氧化铝催化剂上进行的连续方法制备。

6. 发明授权

US6005122A 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
标题翻译：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。

7. 发明授权

US4538009A Preparation of substituted phenols 失效
标题翻译：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。

8. 发明授权

US06784303B2 Method for continuously acylating chromanol ester derivatives 失效
标题翻译：连续酰化色氨酸酯衍生物的方法
公开(公告)号：US06784303B2
公开(公告)日：2004-08-31
申请号：US10416468
申请日：2003-05-12
申请人： Carsten Oost , Gerd Kaibel , Harald Laas , Peter Schmitt , Jens von Erden
发明人： Carsten Oost , Gerd Kaibel , Harald Laas , Peter Schmitt , Jens von Erden
IPC分类号： C07D31176
CPC分类号： C07D311/72 , B01D1/22 , B01D3/009 , B01D3/146 , B01D3/322 , Y02P20/127
摘要： A process is described for continuously preparing chromanol ester derivatives, in particular for continuously preparing carboxylic esters of tocopherols and tocotrienols by continuous acylation with carboxylic acids or carboxylic anhydrides.
摘要翻译：描述了连续制备色甘醇酯衍生物的方法，特别是通过用羧酸或羧酸酐连续酰化连续制备生育酚和生育三烯酚的羧酸酯。

9. 发明授权

US06554965B1 Rectification column for isolating pure substances from high boiling air-and/or temperature sensitive substances 失效
标题翻译：用于从高沸点空气和/或温度敏感物质中分离纯物质的精馏塔
公开(公告)号：US06554965B1
公开(公告)日：2003-04-29
申请号：US09466844
申请日：1999-12-20
申请人： Horst Hartmann , Wolfram Burst , Wulf Kaiser , Harald Laas , Paul Grafen , Bernhard Bockstiegel , Kai-Uwe Baldenius
发明人： Horst Hartmann , Wolfram Burst , Wulf Kaiser , Harald Laas , Paul Grafen , Bernhard Bockstiegel , Kai-Uwe Baldenius
IPC分类号： B01D300
CPC分类号： B01D3/141 , B01D3/008 , B01D3/146 , B01D3/16 , B01J19/32 , B01J2219/3221 , B01J2219/3222 , B01J2219/32227 , B01J2219/32272 , B01J2219/32408 , B01J2219/32416 , B01J2219/326 , C07C17/38 , C07D311/72 , Y10S159/42 , Y10S261/72
摘要： A reflection column which contains liquid distributors having at least 500 drip points/m2, which are arranged at an angle of about 90° C. to cloth layers of packing elements located immediately therebelow; and a combination of insulation and protective heating. The column is advantageously used for the rectification of mixtures of high-boiling air- or temperature-sensitive substances requiring effective separation efficiency.
摘要翻译：一种反射柱，其包含具有至少500个滴点/ m 2的液体分配器，其以约90℃的角度布置在紧邻其下方的包装元件的布层; 并结合绝缘和保护加热。该柱有利地用于需要有效分离效率的高沸点空气或温度敏感物质的混合物的精馏。

10. 发明授权

US06365758B1 Preparation of tocopheral carboxylates or tocotrienyl esters by acid-catalyzed reaction with carboxylic acids 失效
标题翻译：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。

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