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    Production of aminohalogencrotonates
    1.
    发明授权
    Production of aminohalogencrotonates 失效
    生产氨基卤代巴豆酸酯

    公开(公告)号：US06423866B1

    公开(公告)日：2002-07-23

    申请号：US09530909

    申请日：2000-05-08

    申请人： Max Braun ,  Francine Jannssens ,  Werner Rudolph ,  Kerstin Eichholz

    发明人： Max Braun ,  Francine Jannssens ,  Werner Rudolph ,  Kerstin Eichholz

    IPC分类号： C07C22900

    CPC分类号： C07C227/08 ,  C07C229/30

    摘要： Lower alkyl esters of 3-amino crotonates substituted by halogen in the C-4 position, e.g. ethyl 3-amino-4,4,4-trifluoro-crotonate, in which the amino group optionally may be substituted by one or two C1 to C3 alkyl groups or by one or two aryl groups, e.g. phenyl, are synthesized by thermolysis of ammonium salts of corresponding lower alkyl esters of acetoacetic acid substituted in the C-4 position by halogen, and removal of the resulting water of reaction. The water of reaction may be removed by an entraining agent, which preferably has a specific gravity heavier than that of the aqueous phase which forms in the reaction. This minimizes yield losses due to the ammonium salt becoming dissolved in the aqueous phase and results in especially high yields. Formation of the ammonium salt and thermolysis can be carried out simultaneously. Alternatively, it is possible to start from a molten ammonium salt of the halogencrotonate, e.g. the salt of the lower alkyl ester of 4,4,4-trifluoroacetoacetic acid, or to produce the salt in situ, and to pass an inert gas through the molten salt under thermolytic conditions and in the absence of a solvent. In this way the desired product can be produced in high yield and in high purity. This alternative can be implemented as a continuous process.

    摘要翻译： C-4位被卤素取代的3-氨基巴豆酸酯的低级烷基酯，例如 3-氨基-4,4,4-三氟巴豆酸乙酯，其中氨基可任意地被一个或两个C 1至C 3烷基取代，或被一个或两个芳基取代。 苯基，通过用卤素热解在C-4位置取代的乙酰乙酸的相应低级烷基酯的铵盐，除去所得的反应水来合成。 反应水可以通过夹带剂除去，该夹带剂优选具有比在反应中形成的水​​相重的比重。 这使得由于铵盐溶解在水相中导致的产量损失最小化并导致特别高的产率。 铵盐的形成和热解可以同时进行。 或者，可以从卤代克酸内酯的熔融铵盐开始，例如， 4,4,4-三氟乙酰乙酸的低级烷基酯的盐，或者在原位产生盐，并在惰性溶解条件下和不溶于溶剂的条件下使惰性气体通过熔融盐。 以这种方式，可以以高产率和高纯度生产所需的产物。 这种替代方案可以被实现为连续过程。

    Method of making carotenoids
    2.
    发明授权
    Method of making carotenoids 有权
    制备类胡萝卜素的方法

    公开(公告)号：US6150561A

    公开(公告)日：2000-11-21

    申请号：US148088

    申请日：1998-09-04

    申请人： Paul Kreienbuhl ,  Peter Rudin ,  Werner Rudolph

    发明人： Paul Kreienbuhl ,  Peter Rudin ,  Werner Rudolph

    IPC分类号： C07B37/04 ,  C07C1/34 ,  C07C11/02 ,  C07C11/21 ,  C07C45/51 ,  C07C67/31 ,  C07C67/343 ,  C07C69/347 ,  C07C69/602 ,  C07C403/02 ,  C07C403/06 ,  C07C403/16 ,  C07C403/20 ,  C07C403/24 ,  C07C45/00

    CPC分类号： C07C403/24 ,  C07C1/34 ,  C07C403/14 ,  C07C403/20 ,  C07C45/515 ,  C07C67/343 ,  C07C2101/16

    摘要： A widely applicable process for the manufacture of carotenoids by a Wittig reaction comprises carrying out the Wittig reaction in a polar reaction medium in a manner such that neither the reactants nor the thus-manufactured carotenoid are significantly dissolved in the reaction medium. An especially suitable reaction medium is a polar, toxicologically harmless solvent which remains monophasic on the addition of water in an amount up to about 30 vol. % and which permits the triarylphosphine oxide which is formed to dissolve well. Lower alcohols and acetone, as sole solvents or as mixtures with one another and/or with water, are especially suitable as the polar reaction medium. This process permits the use of much more concentrated reaction mixtures, simplifies the regeneration of the solvent and generally the reaction procedure, and avoids toxicologically objectionable solvents such as halogenated hydrocarbons.

    摘要翻译： 用于通过Wittig反应制造类胡萝卜素的广泛应用的方法包括在极性反应介质中进行Wittig反应，使得反应物和由此制得的类胡萝卜素都不会明显地溶解在反应介质中。 特别合适的反应介质是极性，毒理学上无害的溶剂，其在加入至多约30体积的量时保持单相。 ％，这使得形成的三芳基氧化膦容易溶解。 作为唯一溶剂或作为彼此和/或与水的混合物的低级醇和丙酮特别适合作为极性反应介质。 该方法允许使用更浓缩的反应混合物，简化了溶剂的再生和通常的反应过程，并避免了毒理学上令人反感的溶剂如卤代烃。

    Low-melting potassium fluoroaluminate
    3.
    发明授权
    Low-melting potassium fluoroaluminate 失效
    低熔点氟铝酸钾

    公开(公告)号：US5985233A

    公开(公告)日：1999-11-16

    申请号：US948396

    申请日：1997-10-10

    申请人： Heinz-Joachim Belt ,  Ruediger Sander ,  Werner Rudolph

    发明人： Heinz-Joachim Belt ,  Ruediger Sander ,  Werner Rudolph

    IPC分类号： B23K35/363 ,  B23K35/36 ,  C01F7/54 ,  B23K35/34

    CPC分类号： C01F7/54 ,  B23K35/3605

    摘要： The production of a potassium fluoroaluminate having a low melting point, which can be used as a flux when soldering aluminum. The potassium fluoroaluminate is prepared in an aqueous medium from aluminum hydroxide, hydrogen fluoride and potassium hydroxide in a molar ratio of aluminum:fluorine:potassium of approximately 1:5:2. After drying at 80.degree. C. under vacuum, the resulting potassium fluoroaluminate has a differential scanning calorimetry melting point of about 548.degree. C.

    摘要翻译： 生产具有低熔点的氟铝酸钾，其可以在焊接铝时用作焊剂。 氟铝酸钾在水性介质中由氢氧化铝，氟化氢和氢氧化钾以铝：氟：钾的摩尔比为约1:5:2的摩尔比制备。 在80℃真空干燥后，得到的氟铝酸钾的差示扫描量热法熔点约为548℃。

    Difluorochloracetyl, dichloracetyl and trichloracetyl chloride preparation
    5.
    发明授权
    Difluorochloracetyl, dichloracetyl and trichloracetyl chloride preparation 失效
    二氯氯乙酰，二氯乙酰和三氯乙酰氯制备

    公开(公告)号：US5919341A

    公开(公告)日：1999-07-06

    申请号：US981423

    申请日：1997-12-23

    申请人： Max Braun ,  Werner Rudolph ,  Kerstin Eichholz

    发明人： Max Braun ,  Werner Rudolph ,  Kerstin Eichholz

    IPC分类号： C07C51/58 ,  C07C53/48 ,  C07C51/00

    CPC分类号： C07C51/58

    摘要： A process for preparing chlorodifluoroacetyl chloride from 1,1-difluoro-2,2-dichloroethylene and dichloroacetyl chloride from trichloroethylene or 1,1,2,2-tetrachloroethane, in which the starting compounds are continuously reacted in the gaseous phase with oxygen to obtain a photochemical oxidation reaction, chlorine being added as a sensitizer, the reaction mixture being irradiated with light having a wavelength .lambda..gtoreq.280 nm, the reaction preferably being carried out unpressurized. Particularly high yields with height selectivity are achieved by using doped high pressure mercury vapor lamps to irradiate the reaction mixture.

    摘要翻译： PCT No.PCT / EP96 / 02596 371 1997年12月23日第 102（e）1997年12月23日PCT PCT 1997年6月17日PCT公布。 出版物WO97 / 00847 日本1997年1月9日由三氯乙烯或1,1,2,2-四氯乙烷从1,1-二氟-2,2-二氯乙烯和二氯乙酰氯制备氯二氟乙酰氯的方法，其中起始化合物在气态 与氧气相进行光化学氧化反应，加入氯作为敏化剂，反应混合物用波长λ= 280nm的光照射，反应优选进行无压力的处理。 通过使用掺杂的高压汞蒸汽灯来照射反应混合物，实现了具有高度选择性的特别高产率。

    Process for preparing polyfluorochlorocarbonyl chlorides and perfluorocarbonyl chlorides with addition of chlorine
    6.
    发明授权
    Process for preparing polyfluorochlorocarbonyl chlorides and perfluorocarbonyl chlorides with addition of chlorine 失效
    制备多氟氯化碳酰氯和全氟化碳酰氯的方法，加氯

    公开(公告)号：US5569782A

    公开(公告)日：1996-10-29

    申请号：US360026

    申请日：1994-12-20

    申请人： Max Braun ,  Werner Rudolph ,  Kerstin Eichholz

    发明人： Max Braun ,  Werner Rudolph ,  Kerstin Eichholz

    IPC分类号： B01J19/08 ,  C07B61/00 ,  C07C51/58 ,  C07C53/46

    CPC分类号： C07C51/58

    摘要： A process for preparing polyfluorochloro- and perfluorocarbonyl chlorides, for example for preparing perfluoropropionyl chloride, chlorodifluoroacetyl chloride or trifluoroacetyl chloride, in which starting materials are employed which have a CHCl.sub.2 group which is converted to a C(O)Cl group by photochemical oxidation with oxygen in the presence of added elemental chlorine and under exposure to activating irradiation by light having a wavelength .lambda..gtoreq.290 nm. The procedure is preferably unpressurized. Outstanding conversions with high selectivity are achieved using doped Hg light sources.

    摘要翻译： 制备全氟氯代全氟羰基氯的方法，例如用于制备全氟丙酰氯，氯二氟乙酰氯或三氟乙酰氯，其中使用具有CHCl 2基团的起始原料，其通过用氧化物进行光化学氧化转化成C（O）Cl基团 在添加的元素氯的存在下，并且在通过波长λ> 290nm的光的激活照射下曝光。 该方法优选不加压。 使用掺杂的Hg光源实现了高选择性的卓越转化。

    Production of perfluoroalkanes
    7.
    发明授权
    Production of perfluoroalkanes 失效
    生产全氟烷烃

    公开(公告)号：US5434319A

    公开(公告)日：1995-07-18

    申请号：US220003

    申请日：1994-03-30

    申请人： Ralf Herkelmann ,  Werner Rudolph ,  Ruediger Sander ,  Alf Schulz

    发明人： Ralf Herkelmann ,  Werner Rudolph ,  Ruediger Sander ,  Alf Schulz

    IPC分类号： C07C17/10 ,  C07C17/395 ,  C07C19/08

    CPC分类号： C07C17/10 ,  C07C17/395

    摘要： A method for stabilizing and/or purifying perfluoroalkanes, particularly from perfluoroalkanes which contain polyfluoroalkane by-products from their production process, in which the perfluoroalkanes are stabilized and/or purified by reacting the polyfluoroalkane(s) with fluorine at elevated pressure and temperature, to obtain perfluoroalkanes which are substantially free of polyfluoroalkanes. The method has the advantage that the perfluorination takes place rapidly and without significant formation of by-products or decomposition products.

    摘要翻译： 一种稳定和/或纯化全氟烷烃的方法，特别是从其全氟烷烃，其中含有从其制备方法得到的多氟烷烃副产物，其中全氟烷烃在升高的压力和温度下使多氟烷烃与氟反应稳定和/或纯化， 获得基本上不含多氟烷烃的全氟烷烃。 该方法具有以下优点：全氟化快速发生，而不显着形成副产物或分解产物。