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    Preparation of aliphatic, unsaturated nitriles
    1.
    发明授权
    Preparation of aliphatic, unsaturated nitriles 失效
    脂肪族不饱和腈的制备

    公开(公告)号：US5892092A

    公开(公告)日：1999-04-06

    申请号：US144478

    申请日：1998-08-31

    申请人： Andreas Kramer ,  Wolfgang Siegel ,  Michael Henningsen ,  Georg Heinrich Grosch

    发明人： Andreas Kramer ,  Wolfgang Siegel ,  Michael Henningsen ,  Georg Heinrich Grosch

    IPC分类号： B01J23/02 ,  C07B61/00 ,  C07C253/00 ,  C07C255/06 ,  C07C255/07 ,  C07C255/31

    CPC分类号： C07C253/00

    摘要： A process for preparing unsaturated nitriles of the formula I ##STR1## where R, R.sup.1 and R.sup.2 are each independently of one another alkyl or alkenyl each having 1-20 carbon atoms or cycloalkyl or cycloalkenyl each having 3-12 carbon atoms and any two of the radicals R, R.sup.1 and R.sup.2 may be part of a saturated or unsaturated ring and R.sup.1 and R.sup.2 may also be hydrogen and n is 0 or 1-20, by dehydration of oximes of the formula II ##STR2## where R, R.sup.1, R.sup.2 and n are as defined above, comprises dehydrating in the gas or liquid phase at from 150.degree. to 300.degree. C. over a heterogeneous catalyst consisting of an oxidic, carbidic or nitridic support doped with basic oxides and/or hydroxides or compounds which are converted into said oxides or hydroxides under the reaction conditions, or of said basic oxides.

    摘要翻译： 制备式I的不饱和腈的方法，其中R，R 1和R 2各自独立地为各自具有1-20个碳原子的烷基或链烯基或各自具有3-12个碳原子的环烷基或环烯基，任何两个 的基团R 1，R 2和R 2可以是饱和或不饱和环的一部分，R 1和R 2也可以是氢，n是0或1-20，通过式II的肟脱水，其中R，R 1 R2和n如上定义，包括在气相或液相中在150-300℃下脱水，所述非均相催化剂由掺有碱性氧化物和/或氢氧化物或化合物的氧化，碳化或氮化载体组成， 在反应条件下或所述碱性氧化物中转化为所述氧化物或氢氧化物。

    Method for the production of trioxime derivatives
    2.
    发明授权
    Method for the production of trioxime derivatives 失效
    生产三肟衍生物的方法

    公开(公告)号：US06906223B2

    公开(公告)日：2005-06-14

    申请号：US10332046

    申请日：2001-07-04

    申请人： Andreas Kramer ,  Matthias Kiefer ,  Michael Henningsen ,  Wolfgang Siegel ,  Jochen Schröder

    发明人： Andreas Kramer ,  Matthias Kiefer ,  Michael Henningsen ,  Wolfgang Siegel ,  Jochen Schröder

    IPC分类号： C07B61/00 ,  C07C249/06 ,  C07C249/08 ,  C07C251/40 ,  C07C251/58 ,  C07C49/12 ,  C07C251/60

    CPC分类号： C07C249/06 ,  C07C249/08 ,  C07C251/40

    摘要： The present invention relates to a process for preparing trioxime derivatives of the formula I in which the substituents R1 and R2 are identical or different and each is cyano, alkyl, haloalkyl or cycloalkyl, and R3 and R4 are identical or different and each is alkyl, haloalkyl, cycloalkyl, alkylcarbonyl or arylalkyl, by the following reaction steps in water without isolation of the intermediates: A) nitrosation of 1,3-diketones of the formula II  to give monooximes of the formula III, B) oximation of III with hydroxylamine derivatives of the formula IV H2N—OR3′  IV  in which R3′ is hydrogen or a group R3 to give bisoximes of the formula V, C) alkylation of V with alkylating agents or acylation of V with acylating agents to give compounds of the formula VI and D) subsequent oximation of VI with hydroxylamine to give compounds of the formula I.

    摘要翻译： 本发明涉及一种制备式I的三肟衍生物的方法，其中取代基R 1和R 2是相同或不同的，并且各自为氰基，烷基，卤代烷基 或环烷基，R 3和R 4相同或不同，并且各自为烷基，卤代烷基，环烷基，烷基羰基或芳烷基，通过以下反应步骤在水中不分离 中间体：A）式II的1,3-二酮的亚硝化，得到式III的单肟，B）III式与Ⅳ的羟胺衍生物的肟化，其中式Ⅳ的线性公式描述=“在线式 “end =”lead“？> H 2 N-OR 3”在线公式描述=“在线公式”end =“tail” 其中R 3'是氢或基团R 3'，得到式V的双肟，C）用烷基化剂烷基化V或用酰化酰化V 试剂得到式VI化合物和D）随后的肟基 VI与羟胺的离子，得到式I的化合物。

    Process for preparing cyclopropylacetylene
    3.
    发明授权
    Process for preparing cyclopropylacetylene 失效
    环丙基乙炔的制备方法

    公开(公告)号：US06207864B1

    公开(公告)日：2001-03-27

    申请号：US09380382

    申请日：1999-09-01

    申请人： Michael Henningsen ,  Armin Stamm ,  Martin Fischer ,  Wolfgang Siegel

    发明人： Michael Henningsen ,  Armin Stamm ,  Martin Fischer ,  Wolfgang Siegel

    IPC分类号： C07C4530

    CPC分类号： C07F9/535 ,  C07C1/30 ,  C07C17/00 ,  C07C17/18 ,  C07C2601/02 ,  C07C13/04 ,  C07C22/00

    摘要： The invention relates to a process for the halogenation of cyclopropylmethyl ketone with at least one dihalo-triorganophosphorane of the general formula I R3PHal2   (I), in which the radicals R can be the same or different and denote a saturated or unsaturated aliphatic C1-C20 hydrocarbon radical, a phenyl or (C1-C4 alkyl)phenyl radical, which may be optionally substituted by one or two fluorine, chlorine and/or nitro groups, P stands for phosphorus and Hal denotes chlorine, bromine, or iodine, at a temperature of from 800° to 130° C., where the dihalo-triorganophosphane of the general formula (I) is synthesized in situ from triorganophosphane oxide or triorganophosphane sulfide of the general formula II R3PA   (II), in which R is as defined above with respect to formula I and A denotes oxygen or sulfur, using a halogenating agent, wherein the triorganophosphane oxide or triorganophosphane sulfide is used in catalytic amounts, to the halogenation product of cyclopropylmethyl ketone obtained in said process, and to a process for the conversion of said halogenation product to cyclopropylacetytene.

    摘要翻译： 本发明涉及用至少一种通式Iin的二卤代三有机基磷烷卤化环丙基甲基酮的方法，其中基团R可以相同或不同，表示饱和或不饱和的脂族C 1 -C 20烃基，苯基或 （C 1 -C 4烷基）苯基，其可任选被一个或两个氟，氯和/或硝基取代，P代表磷，Hal代表氯，溴或碘，温度为800°至130° ℃，其中通式（I）的二卤代三有机膦原位由通式IIin的三有机膦氧化物或三有机磷烷硫化物原位合成，其中R如对于式I所定义，A表示氧或硫，使用 一种卤化剂，其中三有机膦氧化物或三有机基硫化物以催化量使用于在所述方法中获得的环丙基甲基酮的卤化产物，t o将所述卤化产物转化为环丙基乙烯基的方法。

    Process for the preparation of substituted anthraquinones
    7.
    发明授权
    Process for the preparation of substituted anthraquinones 失效
    制备取代蒽醌的方法

    公开(公告)号：US6127580A

    公开(公告)日：2000-10-03

    申请号：US200936

    申请日：1998-11-30

    申请人： Wolfgang Siegel ,  Andreas Kramer

    发明人： Wolfgang Siegel ,  Andreas Kramer

    IPC分类号： C07C46/02 ,  C07C45/00

    CPC分类号： C07C46/02

    摘要： Process for the preparation of anthraquinones of the general formula I ##STR1## in which R.sup.1, R.sup.2, R.sup.3 and R.sup.4, which can be identical or different, are hydrogen, a C.sub.1 -C.sub.8 -alkyl or C.sub.2 -C.sub.8 -alkenyl radical, in which 1,4-naphthoquinone is reacted with a 1,3-diene of the general formula II ##STR2## in a cycloaddition step to give the corresponding tetrahydroanthraquinone and the tetrahydroanthraquinone is oxidized with oxygen in the presence of a basic catalyst to give the anthraquinone, in which both the cycloaddition step and the oxidation step are carried out in the presence of an aqueous diluent.Preferably, the cycloaddition step and oxidation step are carried out at a reaction temperature between 90 and 110.degree. C. and at atmospheric pressure.

    摘要翻译： 用于制备通式I的蒽醌的方法，其中可以相同或不同的R 1，R 2，R 3和R 4是氢，C 1 -C 8 - 烷基或C 2 -C 8 - 烯基，其中1,4 萘醌在环加成步骤中与通式II的1,3-二烯反应，得到相应的四氢蒽醌，四氢蒽醌在碱性催化剂存在下用氧氧化得到蒽醌，其中环加成步骤 并且氧化步骤在水性稀释剂的存在下进行。 优选环加成步骤和氧化步骤在90-110℃的反应温度和大气压下进行。

    Process for preparing essentially formic acid-free N-alkyl-N′-methylalkyleneureas
    9.
    发明授权
    Process for preparing essentially formic acid-free N-alkyl-N′-methylalkyleneureas 有权
    基本上不含无甲酸的N-烷基-N'-甲基亚烷基脲的方法

    公开(公告)号：US06554966B1

    公开(公告)日：2003-04-29

    申请号：US09603195

    申请日：2000-06-26

    申请人： Andreas Kramer ,  Johann-Peter Melder ,  Heinz Rütter ,  Günter Riewe ,  Wolfgang Siegel ,  Hans-Jürgen Weyer

    发明人： Andreas Kramer ,  Johann-Peter Melder ,  Heinz Rütter ,  Günter Riewe ,  Wolfgang Siegel ,  Hans-Jürgen Weyer

    IPC分类号： B01D300

    CPC分类号： C07D239/10

    摘要： The invention relates to a process for preparing essentially formic acid-free N-alkyl-N′-methylalkyleneureas of the formula with R1=H or CH3, R2=CnH2n+1 with n=1-4 and x=0 or 1, from the corresponding alkyleneureas by reaction with monomeric or polymerized formaldehyde in the presence of formic acid. This entails feeding the mixture, obtained in the reaction, of N-alkyl-N′-methylalkyleneurea and formic acid to the upper region of a distillation column, distilling without further additions and removing essentially formic acid-free N-alkyl-N′-methylalkyleneurea in the lower region of the column. The process parameters are set so that the pressure in the upper region of the column is at a higher level than in the lower region of the column, and the difference in pressure between the upper and lower regions of the column is from 10 to 100 mbar, and the temperature in the lower region of the column is higher than in the upper region of the column, with the difference in temperature between the upper and lower regions of the column being from 40° C. to 210° C.

    摘要翻译： 本发明涉及一种制备基本上无甲酸的N-烷基-N'-甲基亚烷基脲的方法，其中R1 = H或CH3，R2 = CnH2n + 1，其中n = 1-4和x = 0或1， 通过在甲酸存在下与单体或聚合的甲醛反应来制备相应的亚烷基脲。 这需要将N-烷基-N'-甲基亚烷基脲和甲酸的反应混合物加入到蒸馏塔的上部区域，无需进一步添加即可蒸馏除去基本上不含甲酸的N-烷基-N'- 甲基亚烷基脲在柱的下部区域。 设定工艺参数使得塔的上部区域中的压力处于比塔的下部区域更高的水平，并且塔的上部和下部区域之间的压力差为10至100mbar ，塔的下部区域的温度高于塔的上部区域，塔的上部和下部区域之间的温度差为40℃〜210℃。

    Process for preparing ketones, in particular 6-methylheptan-2-one
    10.
    发明授权
    Process for preparing ketones, in particular 6-methylheptan-2-one 失效
    制备酮的方法，特别是6-甲基庚-2-酮

    公开(公告)号：US06303823B2

    公开(公告)日：2001-10-16

    申请号：US09729459

    申请日：2000-12-05

    申请人： Andreas Kramer ,  Christian Knoll ,  Johann-Peter Melder ,  Wolfgang Siegel ,  Gerd Kaibel

    发明人： Andreas Kramer ,  Christian Knoll ,  Johann-Peter Melder ,  Wolfgang Siegel ,  Gerd Kaibel

    IPC分类号： C07C4573

    CPC分类号： C07C45/74 ,  C07C45/62 ,  C07C45/73 ,  C07C49/04 ,  C07C49/203

    摘要： A process for preparing ketones by so-called “crossed aldol condensation” of a ketone with an aldehyde in the presence of a catalyst system consisting of approximately equimolar amounts of a secondary amine and of a carboxylic acid containing at least 2 C atoms, to form an &agr;,&bgr;-unsaturated ketone, and, where appropriate, subsequent catalytic hydrogenation. The process is used in particular for preparing 6-methyl-3-hepten-2-one by reacting acetone with isovaleraldehyde, and for preparing its hydrogenation product, 6-methylheptan-2-one, which is an important precursor for numerous active substances, in particular for preparing lipid-soluble vitamins such as vitamin E.

    摘要翻译： 在由大约等摩尔量的仲胺和含有至少2个C原子的羧酸组成的催化剂体系的存在下，通过所谓的“交叉醛醇缩合”酮与醛制备酮的方法，以形成 α，β-不饱和酮，以及适当的后续催化氢化。该方法特别用于通过丙酮与异戊醛反应制备6-甲基-3-庚烯-2-酮，并用于制备其氢化产物6 - 甲基庚-2-酮，其是许多活性物质的重要前体，特别是用于制备脂溶性维生素如维生素E.