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    Process for the preparation of enantiomerically pure (5, 5′-dichloro-6,6′-dimethoxy-biphenyl-2,2′-diyl)- bis(diphenylphosphine oxides)
    1.
    发明授权
    Process for the preparation of enantiomerically pure (5, 5′-dichloro-6,6′-dimethoxy-biphenyl-2,2′-diyl)- bis(diphenylphosphine oxides) 有权
    制备对映体纯（5，5'-二氯-6,6'-二甲氧基 - 联苯-2,2'-二基） - 双（二苯基膦氧化物）的方法

    公开(公告)号：US06489513B2

    公开(公告)日：2002-12-03

    申请号：US10010176

    申请日：2001-11-13

    申请人： Torsten Pohl ,  Thomas Prinz ,  Guido Giffels ,  Wolfram Sirges

    发明人： Torsten Pohl ,  Thomas Prinz ,  Guido Giffels ,  Wolfram Sirges

    IPC分类号： C07F953

    CPC分类号： C07F9/5329

    摘要： The invention relates to the preparation of enantiomerically pure bis-diphenylphosphine oxides in a particularly advantageous manner by (1) reacting an aromatic bromine compound with a diphenylphosphinic chloride in a mixture of tetrahydrofuran and an aromatic hydrocarbon to give a diphenylphosphine oxide, which is isolated from a solution in an aromatic hydrocarbon by adding a saturated aliphatic hydrocarbon; (2) metalating the resulting diphenylphosphine oxide in the 6-position and reacting the metalated diphenylphosphine oxide with iodine at temperatures not less than −25° C. in such a way that a small amount of iodine is always present in excess, giving a 2-iodo-diphenylphosphine oxide; (3) preparing a racemic bis-diphenylphosphine oxide from the resulting 2-iodo-diphenylphosphine oxide using copper and an aromatic hydrocarbon solvent and crystallizing the racemic bis-diphenylphosphine oxide from a solution in an aromatic hydrocarbon; and (4) separating isomers using an enantiomerically pure mono- or dicarboxylic acid to obtain a first enantiomer by crystallization from a solution in an aromatic hydrocarbon and obtaining a second enantiomer by hydrolysis and subsequent crystallization from a solution in an aromatic hydrocarbon.

    摘要翻译： 本发明涉及通过（1）使芳族溴化合物与二苯基次膦酰氯在四氢呋喃和芳族烃的混合物中反应得到二苯基氧化膦，特别有利的方法制备对映体纯双的二苯基膦氧化物，得到二苯基氧化膦 通过加入饱和脂肪烃在芳族烃中的溶液; （2）将得到的二苯基氧化膦金属化在6位上，并使金属化二苯基氧化膦与碘在不低于-25℃的温度下反应，使得少量的碘总是存在于过量的中，得到2 碘代二苯基氧化膦; （3）使用铜和芳烃溶剂从所得的2-碘 - 二苯基氧化膦制备外消旋二苯基二氧化膦氧化物，并从外来物质中溶解外消旋双 - 二苯基膦氧化物; 和（4）使用对映异构体纯的单羧酸或二羧酸分离异构体，以通过从芳族烃溶液中结晶获得第一对映异构体，并通过水解并随后从芳族烃溶液中结晶得到第二对映异构体。

    Intermediates for the synthesis of bisphosphine compounds
    3.
    发明授权
    Intermediates for the synthesis of bisphosphine compounds 失效
    用于合成双膦化合物的中间体

    公开(公告)号：US5739360A

    公开(公告)日：1998-04-14

    申请号：US714747

    申请日：1996-09-16

    申请人： Wolfram Sirges ,  Christian Laue ,  Dieter Arlt ,  Rolf Grosser

    发明人： Wolfram Sirges ,  Christian Laue ,  Dieter Arlt ,  Rolf Grosser

    IPC分类号： B01J31/16 ,  C07B53/00 ,  C07B57/00 ,  C07B61/00 ,  C07F9/655 ,  C07D307/91

    CPC分类号： C07F9/65517

    摘要： The invention relates to novel bisphosphonates and to processes for their preparation and for their resolution into the enantiomers. The bisphosphonates according to the invention are valuable intermediates for the preparation of bisphosphine compounds, especially chiral bisphosphine ligands. These in turn are constituents of transition metal complexes which are used as catalysts inter alia in asymmetric hydrogenation. The novel bisphosphonates have the general formula (I) ##STR1## in which R.sup.1 is linear or branched alkyl having up to 6 carbon atoms, aryl or aralkyl, each of which can optionally be substituted, or two radicals R.sup.1 together are a bridging hydrocarbon radical having up to 6 carbon atoms, and can exist in the form of their racemates or as enantiomers.

    摘要翻译： 本发明涉及新的双膦酸盐及其制备方法及其分解成对映体。 根据本发明的双膦酸盐是制备双膦化合物，特别是手性双膦配体的有价值的中间体。 这些又是作为催化剂的过渡金属络合物的成分，特别是用于不对称氢化。 新型二膦酸盐具有通式（I）其中R 1为具有至多6个碳原子的直链或支链烷基，芳基或芳烷基，其中每一个可任选被取代，或两个基团R 1一起为 具有至多6个碳原子的桥连烃基，并且可以以其外消旋体的形式存在或作为对映异构体存在。

    Method for producing N-methyl-N′-nitroguanidine
    4.
    发明授权
    Method for producing N-methyl-N′-nitroguanidine 有权
    制备N-甲基-N'-硝基胍的方法

    公开(公告)号：US06720451B2

    公开(公告)日：2004-04-13

    申请号：US10169842

    申请日：2002-07-09

    申请人： Kai van Laak ,  Wolfram Sirges

    发明人： Kai van Laak ,  Wolfram Sirges

    IPC分类号： C07C29100

    CPC分类号： C07C277/08 ,  C07C279/36

    摘要： The present invention relates to a novel process for the preparation of N-methyl-N′-nitroguanidine by reacting nitroguanidine with aqueous methylamine solution buffered by the addition of inorganic or organic acids.

    摘要翻译： 本发明涉及通过硝基胍与加入无机或有机酸缓冲的甲胺溶液反应制备N-甲基-N'-硝基胍的新方法。