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    Preparation of .gamma.,.delta.-unsaturated ketones by the Carroll reaction, novel catalysts therefor and the preparation thereof
    11.
    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。

    Preparation of o,o'-dithiodibenzamides
    12.
    发明授权
    Preparation of o,o'-dithiodibenzamides 失效
    邻二碘苄基酰胺的制备

    公开(公告)号：US4727188A

    公开(公告)日：1988-02-23

    申请号：US717010

    申请日：1985-03-28

    申请人： Hagen Jaedicke

    发明人： Hagen Jaedicke

    IPC分类号： C07C319/24 ,  B01J23/72 ,  C07B61/00 ,  C07C67/00 ,  C07C313/00 ,  C07C323/62 ,  C07C102/00 ,  C07C103/24 ,  C07C103/76 ,  C07C103/78

    CPC分类号： C07C319/24

    摘要： o,o'-Dithiodibenzamides of the formula ##STR1## where R.sup.1 and R.sup.2 are each hydrogen, alkyl or phenyl, R.sup.3 is hydrogen, halogen, nitro, methyl or methoxy, and R.sup.4 has the same meanings as R.sup.3, are prepared by nitrosating an anthranilamide of the formula ##STR2## and reacting the product with sulfur dioxide in the presence of copper or a copper salt.

    摘要翻译： 其中R 1和R 2各自为氢，烷基或苯基，R 3为氢，卤素，硝基，甲基或甲氧基，且R 4具有与R 3相同的化合物，其中R 1和R 2各自为氢，烷基或苯基， 邻氨基苯甲酰胺，并在铜或铜盐存在下使产物与二氧化硫反应。

    Preparation of saccharin
    13.
    发明授权
    Preparation of saccharin 失效
    糖精的制备

    公开(公告)号：US4464537A

    公开(公告)日：1984-08-07

    申请号：US320333

    申请日：1981-11-12

    申请人： Peter Tonne ,  Hagen Jaedicke

    发明人： Peter Tonne ,  Hagen Jaedicke

    IPC分类号： C07D275/06

    CPC分类号： C07D275/06

    摘要： A process for the preparation of saccharin by reacting an aqueous hydrochloric acid solution of o-methoxycarbonylbenzenediazonium chloride with sulfur dioxide, wherein(a) the aqueous diazonium salt solution is reacted with sulfur dioxide at from 0.degree. to 100.degree. C. in the presence of a water-immiscible or only partially water-miscible inert organic solvent,(b) in order to decompose the diazonium salt, the reaction mixture is treated simultaneously or subsequently with a diazonium salt decomposition catalyst,(c) the aqueous organic reaction mixture, or the organic phase obtained after removing the aqueous phase, is treated with an oxidizing agent at from 0.degree. to 100.degree. C. and(d) the organic phase is reacted with aqueous ammonia at from 0.degree. to 50.degree. C. and the saccharin is isolated from the aqueous phase in a conventional manner by acidifying with a strong acid.

    摘要翻译： 通过使邻甲氧基羰基苯并重氮盐酸盐水溶液与二氧化硫反应来制备糖精的方法，其中（a）重氮盐水溶液与二氧化硫在0℃至100℃下，在 （b）为了分解重氮盐，将反应混合物同时或随后用重氮盐分解催化剂处理，或（c）含水有机反应混合物，或 除去水相后得到的有机相用0〜100℃的氧化剂处理。

    Process for preparing unsaturated ketones
    15.
    发明授权
    Process for preparing unsaturated ketones 失效
    制备不饱和酮的方法

    公开(公告)号：US06307106B1

    公开(公告)日：2001-10-23

    申请号：US09440280

    申请日：1999-11-15

    申请人： Carsten Oost ,  Manfred Stroezel ,  Heinz Etzrodt ,  Dietmar Weller ,  Gerd Kaibel ,  Hagen Jaedicke

    发明人： Carsten Oost ,  Manfred Stroezel ,  Heinz Etzrodt ,  Dietmar Weller ,  Gerd Kaibel ,  Hagen Jaedicke

    IPC分类号： C07C4500

    CPC分类号： C07C45/68 ,  B01J19/1881 ,  B01J31/0211 ,  B01J2219/00038 ,  Y02P20/582 ,  C07C49/203

    摘要： An improved process for preparing lower unsaturated ketones by reacting the corresponding &agr;,&bgr;-unsaturated alcohols with alkyl acetoacetates in a Carroll reaction in the presence of from 0.1 to 5 mol %, based on the alkyl acetoacetate to be reacted, of an organic aluminum compound as catalyst with elimination and continuous removal by distillation of the alkanol eliminated during the reaction from the alkyl acetoacetate in a reactor system with a fitted fractionation column, wherein A an &agr;,&bgr;-unsaturated alcohol which boils below 140° C. is introduced, in the absence of effective amounts of a solvent, together with the organic aluminum compound into the reaction vessel, B a reaction temperature which is as constant as possible between 170° C. and 250° C. is set under elevated pressure, C at this temperature, the alkyl acetoacetate is metered into the mixture, obtained in A, of the &agr;,&bgr;-unsaturated alcohol and the organic aluminum compound, and D during the reaction the content of alkyl acetoacetate in the reaction mixture is set at a value which is as constant as possible between 0.1 and 10% by weight.

    摘要翻译： 一种改进的制备低级不饱和酮的方法，该方法通过在卡罗尔反应中使相应的α，β-不饱和醇与烷基乙酰乙酸酯在0.1至5摩尔％存在下反应的待反应的乙酰乙酸烷基酯的有机铝化合物 作为催化剂，在具有适合的分馏塔的反应器系统中通过蒸馏从乙酰乙酸烷基酯反应中消除的烷醇消除并连续除去，其中引入沸点低于140℃的α，β-不饱和醇，在 没有有效量的溶剂与有机铝化合物一起进入反应容器B中，在170℃和250℃之间的反应温度一直保持在升高的压力下，在此温度下， 将乙酰乙酸烷基酯计量加入到A，得自α，β-不饱和醇和有机铝化合物的混合物中，并且在反应期间将D 将反应混合物中乙酰乙酸烷基酯的含量设定为0.1至10重量％之间尽可能恒定的值。

    Preparation of polyenes
    16.
    发明授权
    Preparation of polyenes 失效
    多烯的制备

    公开(公告)号：US5276209A

    公开(公告)日：1994-01-04

    申请号：US914128

    申请日：1992-07-17

    申请人： Hagen Jaedicke ,  Klaus Kaiser ,  Manfred Hamm

    发明人： Hagen Jaedicke ,  Klaus Kaiser ,  Manfred Hamm

    IPC分类号： C07C403/06 ,  C07C45/60 ,  C07C67/02 ,  C07C403/00 ,  C07C403/10 ,  C07C403/12 ,  C07C403/14 ,  C07C403/20 ,  C07C403/22 ,  C07D319/06

    CPC分类号： C07C403/12 ,  C07C403/08 ,  C07C403/14 ,  C07C403/22 ,  C07C45/60 ,  C07D319/06 ,  C07C2101/16

    摘要： An improved process for the preparation of polyenes by the Julia reaction comprises carrying out the allylation of the anion of an allyl aryl sulfone generated a strong base, and the elimination of arylsulfinic acid to form a double bond in the same inert polar solvent which is immiscible with water, preferably in a ketone of the formula IR.sup.1 --CO--R.sup.2 (I)where R.sup.1 and R.sup.2 are each straight-chain or branched alkyl of 2 to 4 carbons, or R.sup.1 and R.sup.2 together are tetramethylene or pentamethylene. The process is particularly important for the preparation of vitamin A derivatives. In the preparation of vitamin A aldehyde, for example, it is advantageous to use the same alkali metal alcoholate as strong base in both stages so that the conversion can be carried out as one-pot reaction.

    摘要翻译： 通过Julia反应制备多烯的改进方法包括进行产生强碱的烯丙基芳基砜的阴离子的烯丙基化，以及消除芳基亚磺酸在与不混溶的相同惰性极性溶剂中形成双键 其中R1和R2分别是2至4个碳的直链或支链烷基，或者R1和R2一起是四亚甲基或五亚甲基。 该方法对于制备维生素A衍生物尤为重要。 在维生素A醛的制备中，例如，在两个阶段中使用相同的碱金属醇盐作为强碱是有利的，因此转化可以作为一锅反应进行。

    Preparation of o,o'-dithiodibenzoic acids
    17.
    发明授权
    Preparation of o,o'-dithiodibenzoic acids 失效
    邻二硫代苯甲酸的制备

    公开(公告)号：US4493802A

    公开(公告)日：1985-01-15

    申请号：US455806

    申请日：1983-01-05

    申请人： Hagen Jaedicke ,  Peter Tonne

    发明人： Hagen Jaedicke ,  Peter Tonne

    IPC分类号： C07C319/14 ,  C07C20060101 ,  C07C67/00 ,  C07C313/00 ,  C07C319/24 ,  C07C323/62 ,  C07C323/66 ,  C07C143/52 ,  C07C149/40

    CPC分类号： C07C319/24

    摘要： o,o'-Dithiodibenzoic acids are prepared by a process wherein a diazotized anthranilic acid or anthranilate is reacted with sulfur dioxide in the presence of an acid, water and a copper salt, and if desired in the presence of an alkali metal iodide, in a 1st stage at from 20.degree. to 50.degree. C. and then in a 2nd stage at from 80.degree. to 100.degree. C.The o,o'-dithiodibenzoic acids obtainable by the process of the invention are useful starting materials for the preparation of crop protection agents, dyes and drugs.

    摘要翻译： o，邻二硫代二苯甲酸是通过一种方法制备的，其中重氮化邻氨基苯甲酸或邻氨基苯甲酸酯在酸，水和铜盐存在下与二氧化硫反应，如果需要，在碱金属碘化物的存在下， 在20℃至50℃的第一阶段，然后在80℃至100℃的第二阶段。通过本发明的方法获得的邻二硫代二苯甲酸是制备 作物保护剂，染料和药物。

    Preparation of aromatic sulfohalides
    20.
    发明授权
    Preparation of aromatic sulfohalides 失效
    芳香族磺酰卤的制备

    公开(公告)号：US4393211A

    公开(公告)日：1983-07-12

    申请号：US320334

    申请日：1981-11-12

    申请人： Peter Tonne ,  Hagen Jaedicke

    发明人： Peter Tonne ,  Hagen Jaedicke

    IPC分类号： C07B61/00 ,  B01J27/00 ,  B01J27/10 ,  B01J31/00 ,  B01J31/02 ,  C07C67/00 ,  C07C301/00 ,  C07C303/02 ,  C07C309/86 ,  C07D215/36 ,  C07C143/70

    CPC分类号： C07C309/00

    摘要： A process for the preparation of aromatic sulfohalides by reacting an aqueous solution, containing a hydrogen halide, of an aromatic diazonium halide with sulfur dioxide, wherein(a) the aqueous solution, containing the hydrogen halide, of a diazonium salt which is derived from the corresponding aromatic amine and the halogen of the desired sulfohalide is reacted with sulfur dioxide in the presence of an inert organic solvent which is immiscible or only partially miscible with water,(b) the diazonium salt is decomposed, simultaneously or subsequently, by means of a catalyst for diazonium salt decomposition and(c) the resulting reaction mixture, or the organic phase thereof after removal of the aqueous phase, is treated with an oxidizing agent.

    摘要翻译： 一种通过使芳族重氮卤化物的水溶液与二氧化硫反应制备芳族磺酰卤的方法，其中（a）含有卤化氢的含有衍生自重氮盐的重氮盐的水溶液 相应的芳香胺和所需磺酰卤的卤素与二氧化硫在惰性有机溶剂的存在下反应，惰性有机溶剂是不混溶的或仅与水部分混溶，（b）重氮盐同时或随后通过 用于重氮盐分解的催化剂和（c）所得反应混合物或其除去水相后的有机相用氧化剂处理。