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    Methods of producing phosphitylated compounds
    5.
    发明授权
    Methods of producing phosphitylated compounds 失效
    磷酸化化合物的制备方法

    公开(公告)号：US07217814B2

    公开(公告)日：2007-05-15

    申请号：US10990138

    申请日：2004-11-16

    申请人： Christian Werner ,  Frank Nerenz ,  Andreas Kanschik-Conradsen ,  Kalakota S. Reddy

    发明人： Christian Werner ,  Frank Nerenz ,  Andreas Kanschik-Conradsen ,  Kalakota S. Reddy

    IPC分类号： C07H21/00

    CPC分类号： C07H19/10 ,  C07H19/20

    摘要： Provided are methods of producing phosphitylated compounds, including 3′-O-phosphoramidites, comprising the step of reacting a hydroxyl-containing compound with a phosphitylating agent in the presence of a phosphitylation activator selected from the group consisting of: (1) acid-base complexes derived from an amine base of Formula II wherein R3, R4, R5, R6, and R7 are independently hydrogen, C1–C10 alkyl, C3–C10 cycloalkyl, C6–C10 aryl, C7–C10 aralkyl, C1–C10 heteroalkyl, or C1–C10 heteroaryl, and at least one of R3, R4, R5, R6, and R7 is not hydrogen; (2) zwitterionic amine complexes; and (3) combinations of two or more thereof, to produce a phosphitylated compound. Further provided are methods for purifying phosphitylated compounds comprising the steps of providing a phosphitylated compound in a solution solvent, contacting said phosphitylated compound with a precipitation solvent, and precipitating said phosphitylated compound.

    摘要翻译： 提供了生产磷酸化化合物（包括3'-O-亚磷酰胺）的方法，包括在含磷酸化活化剂存在下使含羟基的化合物与磷酸化剂反应的步骤，所述磷化活化剂选自：（1）酸碱 衍生自式II的胺碱的络合物，其中R 3，R 4，R 5，R 6， R 7独立地是氢，C 1 -C 10烷基，C 3 -C 10烷基，C 1 -C 10烷基，C 3 -C 10烷基， 环烷基，C 6 -C 10芳基，C 7 -C 10芳烷基，C 1 -C 10烷基， 或者C 1 -C 10杂芳基，以及至少一个R 1，R 2，R 2， R 4，R 4，R 5，R 6和R 7不是氢; （2）两性离子胺络合物; 和（3）两种或更多种的组合，以产生磷酸化化合物。 还提供了纯化磷酸化化合物的方法，包括以下步骤：在溶液中提供磷酸化化合物，使所述磷酸化化合物与沉淀溶剂接触，并使所述磷酸化化合物沉淀。

    Process for the Kumada coupling reaction
    6.
    发明授权
    Process for the Kumada coupling reaction 失效
    Kumada偶联反应的方法

    公开(公告)号：US07205414B2

    公开(公告)日：2007-04-17

    申请号：US11033573

    申请日：2005-01-12

    申请人： Christian Werner ,  Frauke Platz ,  Andreas Kanschik-Conradsen

    发明人： Christian Werner ,  Frauke Platz ,  Andreas Kanschik-Conradsen

    IPC分类号： C07D333/08 ,  C07D333/28

    CPC分类号： C07D333/06

    摘要： A method for the formation of 3-alkylthiophenes or 3-arylthiophenes from 3-halothiophenes. More particularly, improvements on the Kumada coupling reaction for the production of 3-alkylthiophenes or 3-arylthiophenes by reacting a 3-halothiophene with an alkylmagnesiumhalide or arylmagnesiumhalide Grignard reagent in the presence of a catalyst and a 2-methyl tetrahydrofuran solvent. The 2-methyl tetrahydrofuran solvent allows for higher concentrations of the Grignard reagent with minimal or no dithienyl side product generation, achieving higher product yields and at a lower cost than other known methods.

    摘要翻译： 从3-卤代噻吩形成3-烷基噻吩或3-芳基噻吩的方法。 更具体地，通过在催化剂和2-甲基四氢呋喃溶剂的存在下使3-卤代噻吩与烷基镁卤化物或芳基镁卤化物格氏试剂反应制备3-烷基噻吩或3-芳基噻吩的Kumada偶联反应的改进。 2-甲基四氢呋喃溶剂允许较高浓度的格利雅试剂与最少或没有二噻吩基产物的产生相比，获得更高的产物产率并以比其它已知方法更低的成本。

    Methods of producing phosphitylated compounds
    7.
    发明授权
    Methods of producing phosphitylated compounds 失效
    磷酸化化合物的制备方法

    公开(公告)号：US06894158B2

    公开(公告)日：2005-05-17

    申请号：US10373336

    申请日：2003-02-24

    申请人： Christian Werner ,  Frank Nerenz ,  Andreas Kanschik-Conradsen ,  Kalakota Reddy

    发明人： Christian Werner ,  Frank Nerenz ,  Andreas Kanschik-Conradsen ,  Kalakota Reddy

    IPC分类号： C12N15/09 ,  C07B61/00 ,  C07H19/073 ,  C07H19/10 ,  C07H19/173 ,  C07H19/20 ,  C07H21/00

    CPC分类号： C07H19/10 ,  C07H19/20

    摘要： Provided are methods of producing phosphitylated compounds, including 3′-O-phosphoramidites, comprising the step of reacting a hydroxyl-containing compound with a phosphitylating agent in the presence of a phosphitylation activator selected from the group consisting of: (1) acid-base complexes derived from an amine base of Formula I wherein R, R1, and R2 are independently C1-C10 alkyl, C3-C10 cycloalkyl, C6-C10 aryl, C7-C10 aralkyl, C1-C10 heteroalkyl, or C1-C10 heteroaryl, wherein any two adjacent R, R1, and R2 may be connected to form a heterocyclic ring; (2) acid-base complexes derived from a diazabicyclo amine base; and (3) combinations of two or more thereof.

    摘要翻译： 提供了生产磷酸化化合物（包括3'-O-亚磷酰胺）的方法，包括在磷酸化活化剂存在下使含羟基的化合物与磷酸化剂反应的步骤，所述磷化活化剂选自：（1）酸碱 衍生自式I的胺碱的络合物，其中R 1，R 2和R 2独立地为C 1 -C 10烷基， C 1 -C 6烷基，C 3 -C 10环烷基，C 6 -C 10芳基，C

    Low pressure process for the preparation of methanedisulfonic acid alkali metal salts
    8.
    发明申请
    Low pressure process for the preparation of methanedisulfonic acid alkali metal salts 审中-公开
    用于制备甲基二磺酸碱金属盐的低压法

    公开(公告)号：US20060155142A1

    公开(公告)日：2006-07-13

    申请号：US11033580

    申请日：2005-01-12

    申请人： Christian Werner ,  Andreas Kanschik-Conradsen ,  Michael Hoffmeister ,  Harald Heuduk ,  Thomas Scholten

    发明人： Christian Werner ,  Andreas Kanschik-Conradsen ,  Michael Hoffmeister ,  Harald Heuduk ,  Thomas Scholten

    IPC分类号： C07C309/00

    CPC分类号： C07C303/32 ,  C07C303/02 ,  C07C309/05

    摘要： The invention provides a process for producing alkylpolysulfonic acid alkali metal salts such as methanedisulfonic acid alkali metal salts. The process involves heating an aqueous solution of about two molar equivalents of an alkali metal sulfite to a temperature of from about 70° C. to about 90° C.; adding about one molar equivalent of a dihaloalkane to the aqueous alkali metal sulfite solution at a temperature of about 70-90° C.; and then separating the resulting alkyldisulfonic acid alkali metal salt from the reaction solution. The dihaloalkane is added at a pressure of about 1.1 atmospheres or less.

    摘要翻译： 本发明提供了生产烷基聚磺酸碱金属盐如甲基二磺酸碱金属盐的方法。 该方法包括将约2摩尔当量碱金属亚硫酸盐的水溶液加热至约70℃至约90℃的温度; 在约70-90℃的温度下向碱金属亚硫酸盐水溶液中加入约1摩尔当量的二卤代烷烃; 然后从反应溶液中分离得到的烷基二磺酸碱金属盐。 在约1.1大气压或更低的压力下加入二卤代烷烃。

    Process for isomerization of 2-halothiophene to 3-halothiophene
    9.
    发明申请
    Process for isomerization of 2-halothiophene to 3-halothiophene 失效
    2-卤代噻吩异构化为3-卤代噻吩的方法

    公开(公告)号：US20060155133A1

    公开(公告)日：2006-07-13

    申请号：US11033572

    申请日：2005-01-12

    申请人： Christian Werner ,  Andreas Kanschik-Conradsen ,  Bernd Kellermeier ,  Hans-Jurgen Schmidt

    发明人： Christian Werner ,  Andreas Kanschik-Conradsen ,  Bernd Kellermeier ,  Hans-Jurgen Schmidt

    IPC分类号： C07D333/28

    CPC分类号： C07D333/28

    摘要： An improved process and catalyst system for the isomerization of halothiophenes. More particularly, an improved process for the isomerization of 2-halothiopehenes to 3-halothiophenes by reacting a 2-halothiophene with a catalyst and in the presence of a base. The addition of a base additive to the acidic zeolite catalyst allows the desired isomerization reaction to take place while suppressing side-reactions that result in the decomposition of thiophene rings. The catalyst lifetime is thus increased and the amount of catalyst needed for the reaction is reduced, lowering cost.

    摘要翻译： 用于卤代噻吩异构化的改进的方法和催化剂体系。 更具体地说，通过使2-卤代噻吩与催化剂反应并在碱的存在下将2-卤代噻吩异构化成3-卤代噻吩的改进方法。 向酸性沸石催化剂中添加碱添加剂允许发生所需的异构化反应，同时抑制导致噻吩环分解的副反应。 因此催化剂寿命增加，反应所需的催化剂用量降低，成本降低。