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    Racemization of atropisomeric bis(phosphine oxide) compounds
    1.
    发明授权
    Racemization of atropisomeric bis(phosphine oxide) compounds 有权
    无规异构双（氧化膦）化合物的外消旋化

    公开(公告)号：US06288280B1

    公开(公告)日：2001-09-11

    申请号：US09594643

    申请日：2000-06-15

    申请人： Frank Kienzle ,  Michel Lalonde ,  Rudolf Schmid ,  Shaoning Wang

    发明人： Frank Kienzle ,  Michel Lalonde ,  Rudolf Schmid ,  Shaoning Wang

    IPC分类号： C07F953

    CPC分类号： C07F9/5329 ,  C07F9/5054

    摘要： A process for the racemization of atropisomeric bis(phosphine oxide) compounds of formula I: in their (S) or (R) or non-racemic form, is useful for preparing optical active bisphosphine ligands, that form optical active complexes with transition metals. Racemization is thermal and carried out in high or low boiling solvent, under normal or elevated pressure at 105 to 3.5×107 Pa. Heating is performed in a system that allows heating up to 400° C. (reactor, autoclave, aluminum block, round-bottom flask with heating/stirring mantle and the like) or by microwave irradiation or in the melt at a temperature from 260 to 400° C.

    摘要翻译： 式（I）或（R）或非外消旋形式的式I的阻转异构双（氧化膦）化合物外消旋化的方法可用于制备与过渡金属形成光学活性配合物的光学活性双膦配体。 外消旋化是热和在高沸点溶剂或低沸点溶剂中，在正常或升高的压力下，在105-3.5×10 7 Pa下进行，在允许加热到400℃的系统中进行加热（反应器，高压釜，铝块， 具有加热/搅拌罩等的底烧瓶）或通过微波照射或在260-400℃的温度下在熔体中进行。

    Process for the preparation of enantiomerically pure (5, 5′-dichloro-6,6′-dimethoxy-biphenyl-2,2′-diyl)- bis(diphenylphosphine oxides)
    3.
    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。

    Organometallic monoacylarylphosphines
    5.
    发明授权
    Organometallic monoacylarylphosphines 失效
    有机金属一酰基芳基膦

    公开(公告)号：US06399805B2

    公开(公告)日：2002-06-04

    申请号：US09776657

    申请日：2001-02-05

    申请人： Jean-Pierre Wolf ,  Beat Michael Aebli ,  Gebhard Hug

    发明人： Jean-Pierre Wolf ,  Beat Michael Aebli ,  Gebhard Hug

    IPC分类号： C07F953

    CPC分类号： C09D11/101 ,  A61K6/0052 ,  A61K6/08 ,  B33Y70/00 ,  C07F9/28 ,  C07F9/5036 ,  C07F9/5337 ,  C07F9/6521 ,  C08F2/50 ,  C09D4/00 ,  G03F7/0045 ,  G03F7/029 ,  G03F7/0384 ,  G03F7/0388 ,  G03F7/0755 ,  Y10S430/124 ,  A61K6/083 ,  C08L33/08 ,  C08L33/10 ,  C08L33/20 ,  C08L33/26 ,  C08L27/00 ,  C08L31/04 ,  C08L25/06 ,  C08L27/04 ,  C08L39/06 ,  A61K6/09 ,  C08L75/04 ,  A61K6/087 ,  C08L67/00 ,  C08L71/02 ,  A61K6/097 ,  C08L1/08

    摘要： Compounds of the formula I R1 and R2 independently of one another are C1-C20alkyl, OR11, CF3 or halogen; R3, R4 and R5 independently of one another are hydrogen, C1-C20alkyl, OR1 or halogen; R6, R7, R8, R9 and R10 independently of one another are hydrogen, C1-C20alkyl; C2-C20alkyl which is interrupted once or more than once by nonconsecutive O atoms and which is unsubstituted or substituted by OH and/or SH; or R6, R7, R8, R9 and R10 are OR11, SR11, N(R12)(R13), phenyl or halogen; R11 is C1-C20alkyl, C3-C8cycloalkyl, phenyl, benzyl or C2-C20alkyl which is interrupted once or more than once by O or S and which is unsubstituted or substituted by OH and/or SH; R12 and R13 independently of one another are hydrogen, C1-C20alkyl, C3-C8cycloalkyl, phenyl, benzyl or C2-C20alkyl which is interrupted once or more than once by nonconsecutive O atoms and which is unsubstituted or substituted by OH and/or SH; or R12 and R13 together are C3-C5alkylene which can be interrupted by O, S or NR14; R14 is hydrogen, phenyl, C1-C12alkyl or C2-C12alkyl which is interrupted once or more than once by O or S and which is unsubstituted or substituted by OH and/or SH; and M is hydrogen, Li, Na or K; are valuable intermediates for the preparation of unsymmetrical bisacylphosphine oxides and monoacylphosphine oxides.

    摘要翻译： 式IR1和R2的化合物彼此独立地为C1-C20烷基，OR11，CF3或卤素; R 3，R 4和R 5彼此独立地是氢，C 1 -C 20烷基，OR 1或卤素; R 6，R 7，R 8，R 9和R 10彼此独立地是氢，C 1 -C 20烷基; 被不连续的O原子中断一次或多于一次且未被取代或被OH和/或SH取代的C 2 -C 20烷基; 或R 6，R 7，R 8，R 9和R 10为OR 11，SR 11，N（R 12）（R 13），苯基或卤素; R 11是被O或S间隔一次或多于一次并且未被取代或被OH和/或SH取代的C 1 -C 20烷基，C 3 -C 8环烷基，苯基，苄基或C 2 -C 20烷基。 R 12和R 13彼此独立地是氢，C 1 -C 20烷基，C 3 -C 8环烷基，苯基，苄基或C 2 -C 20烷基，其被非连续的O原子中断一次或多于一次，并且是未取代的或被OH和/或SH取代; 或R 12和R 13一起是可被O，S或NR14中断的C 3 -C 5亚烷基; R 14是氢，苯基，C 1 -C 12烷基或C 2 -C 12烷基，其被O或S间隔一次或多于一次，并且是未取代的或被OH和/或SH取代; M为氢，Li，Na或K; 是制备不对称双酰基氧化膦和单酰基氧化膦的有价值的中间体。

    Triarylphosphine oxide derivatives containing fluorine substituents
    7.
    发明授权
    Triarylphosphine oxide derivatives containing fluorine substituents 有权
    含氟取代基的三芳基氧化膦衍生物

    公开(公告)号：US06342638B1

    公开(公告)日：2002-01-29

    申请号：US09695070

    申请日：2000-10-25

    申请人： Tae-Ho Yoon ,  Kwang Un Jeong

    发明人： Tae-Ho Yoon ,  Kwang Un Jeong

    IPC分类号： C07F953

    CPC分类号： C08G73/1057 ,  C07F9/5325

    摘要： The invention relates to triarylphosphine oxide derivatives containing fluorine substituents that are useful as a monomer in preparation of polymers with improved properties such as chemical resistance and electrical insulating property as well as adhesiveness and flame retardancy. The triarylphosphine oxide derivatives containing fluorine substituents are represented by the chemical formula 1: wherein R1 and R2 are independently a fluorine-substituted alkyl group; and X is hydrogen, a nitro group, or an amine group.

    摘要翻译： 本发明涉及含氟取代基的三芳基氧化膦衍生物，其可用作制备具有改进性能如耐化学性和电绝缘性以及粘合性和阻燃性的聚合物的单体。 含氟取代基的三芳基氧化膦衍生物由化学式1表示：其中R1和R2独立地是氟取代的烷基; X为氢，硝基或胺基。