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    Method for producing bridged manganese complexes of triazacyclononane
    1.
    发明授权
    Method for producing bridged manganese complexes of triazacyclononane 有权
    三氮杂环壬烷桥联锰配合物的制备方法

    公开(公告)号：US09012630B2

    公开(公告)日：2015-04-21

    申请号：US13394968

    申请日：2010-09-10

    Applicant: Gerd Reinhardt ,  Michael Best ,  Christian Sidot

    Inventor： Gerd Reinhardt ,  Michael Best ,  Christian Sidot

    IPC: C07F13/00 ,  B01J31/18 ,  B01J31/22

    CPC classification number: C07F13/005 ,  B01J31/182 ,  B01J31/2208 ,  B01J2531/0216

    Abstract: The invention relates to a method for producing manganese complex compounds of the general formula (1), wherein M, X, L, z, Y and q are defined as in claim 1. The method is characterized by the following steps: a) reacting one or more bivalent metal salts with the ligand L in water as the solvent to form a coordination compound from the one or more bivalent metal salt and the ligand L, the one or more bivalent metal salts being selected from bivalent manganese salts and iron salts and at least one bivalent metal salt being a bivalent manganese salt, b) oxidizing the coordination compound of step a) with an oxidant while at the same time maintaining a pH of 11 to 14, to transform the metal M from the bivalent to the trivalent and/or tetravalent form, c) reducing the pH of the reaction mixture to a pH of 4 to 9 and removing any metal oxides or metal hydroxides of the metal M formed and d) adding, at a pH of 4 to 9, a salt of the formula MezYq, wherein Me represents an alkali metal ion, ammonium ion or an alkanol ammonium ion, and Y, z and q are defined as in formula (1).

    Abstract translation: 本发明涉及一种制备通式（1）的锰络合物的方法，其中M，X，L，Z，Y和q如权利要求1中所定义。该方法的特征在于以下步骤：a） 一种或多种二价金属盐与水中的配体L作为溶剂，以从一种或多种二价金属盐和配体L形成配位化合物，一种或多种二价金属盐选自二价锰盐和铁盐，以及 至少一种二价金属盐是二价锰盐，b）用氧化剂氧化步骤a）的配位化合物，同时保持pH为11至14，以将金属M从二价转化成三价和 /或四价形式，c）将反应混合物的pH降低至4至9的pH，并除去形成的金属M的任何金属氧化物或金属氢氧化物，以及d）在pH4至9的条件下，加入 式MezYq，其中Me表示碱金属离子，a 铵离子或烷醇铵离子，Y，Z和q如式（1）所定义。

    Meso-selective synthesis of ansa-metallocenes
    3.
    发明授权
    Meso-selective synthesis of ansa-metallocenes 有权

    公开(公告)号：US07635783B2

    公开(公告)日：2009-12-22

    申请号：US10583574

    申请日：2004-12-15

    Applicant: Reynald Chevalier ,  Patrik Müller ,  Christian Sidot ,  Christian Tellier ,  Valerie Garcia ,  Ludovic Delancray

    Inventor： Reynald Chevalier ,  Patrik Müller ,  Christian Sidot ,  Christian Tellier ,  Valerie Garcia ,  Ludovic Delancray

    IPC: C07F17/00 ,  B01J31/00

    CPC classification number: C07F17/00 ,  C08F10/00 ,  C08F110/06 ,  Y10S526/943 ,  C08F4/65927

    Abstract: The present invention relates to a process for the meso-selective preparation of ansa-metallocene complexes of the formula (I), which comprises reacting a ligand starting compound of the formula (II) with a transition metal compound of the formula III, where R1, R1 are identical or different and are each hydrogen or an organic radical having from 1 to 40 carbon atoms, R2, R2 are identical or different and are each hydrogen or an organic radical having from 1 to 40 carbon atoms, R3 is a bulky organic radical which has at least 3 carbon atoms, is bound to the oxygen atom via a nonaromatic carbon or silicon atom and may be substituted by halogen atoms or further organic radicals having from 1 to 20 carbon atoms and may also contain heteroatoms selected from the group consisting of Si, N, P, O and S, T, T′ are identical or different and are each a divalent organic group which has from 1 to 40 carbon atoms and together with the cyclopentadienyl ring forms at least one further saturated or unsaturated, substituted or unsubstituted ring system having a ring size of from 5 to 12 atoms, where T and T′ may contain the heteroatoms Si, Ge, N, P, As, Sb, O, S, Se or Te within the ring system fused to the cyclopentadienyl ring, A is a bridge consisting of a divalent atom or a divalent group, M1 is an element of group 3, 4, 5 or 6 of the Periodic Table of the Elements or the lanthanides, the radicals X are identical or different and are each an organic or inorganic radical which is able to be replaced by a cyclopentadienyl anion, x is a natural number from 1 to 4, M2 is an alkali metal, an alkaline earth metal or a magnesium monohalide fragment, p is 1 in the case of doubly positively charged metal ions or 2 in the case of singly positively charged metal ions or metal ion fragments, LB is an uncharged Lewis base ligand, and y is a natural number from 0 to 6, and also the subsequent reaction of these complexes to form ansa-metallocenes of the formula (IV), the use of transition metal compounds of the formula (III) for preparing metallocenes and also transition metal compounds of the formula (III), ansa-metallocene complexes of the formula (I) and the use of these as constituents of catalyst systems for the polymerization of olefines.

    Method For Producing 3,7-Diaza-bicyclo[3.3.1]nonane metal complexes
    5.
    发明申请
    Method For Producing 3,7-Diaza-bicyclo[3.3.1]nonane metal complexes 有权
    制备3,7-二氮杂双环[3.3.1]壬烷金属络合物的方法

    公开(公告)号：US20140114073A1

    公开(公告)日：2014-04-24

    申请号：US13877567

    申请日：2011-10-06

    Applicant: Christian Sidot ,  Audrey Caron ,  Miriam Ladwig ,  Gerd Reinhardt

    Inventor： Christian Sidot ,  Audrey Caron ,  Miriam Ladwig ,  Gerd Reinhardt

    IPC: C07F15/02 ,  C07F13/00

    CPC classification number: C07F15/02 ,  C07F13/00 ,  C07F13/005 ,  C07F15/025

    Abstract: The invention relates to a method for producing metal complexes of formula (2) [MaLxXn]Ym (2), where M is a metal from the group consisting of Mn(II), Mn(III), Mn(IV), Fe(II), Fe(III) or Fe(IV), X is a coordinating compound selected from mono-, bi- or tri-charged anions or neutral molecules which can coordinate to a metal in mono-, bi- or tri-dentate form, Y represents a non-coordinating counter-ion which ensures charge equalization of the complex, L represents a ligand of formula (1) or the protonized or de-protonized form thereof, and a, x, n, m, R, R1, R2, R3 and z have the meanings described in claim 1. Said method is characterized in that the reaction of one or more ligands of formula (1) with an iron salt or manganese salt is carried out in an acetone/water mixture in a temperature range from 0 to 50° C. and for this purpose a solution or a suspension of the one or more ligands of formula (1) in acetone is brought in contact with an aqueous metal salt solution of the iron salt or manganese salt in the temperature range in which the reaction takes place.

    Abstract translation: 本发明涉及一种制备式（2）[MaLxXn] Ym（2）的金属配合物的方法，其中M是由Mn（II），Mn（III），Mn（IV），Fe（ II），Fe（III）或Fe（IV），X是选自单，双或三电荷阴离子或中性分子的配位化合物，其可以以单，双或三齿形式与金属配位 ，Y表示非配位抗衡离子，其确保络合物的电荷均衡，L表示式（1）的配体或其质子化或去质子化形式，和a，x，n，m，R，R 1， R2，R3和z具有权利要求1所述的含义。所述方法的特征在于，式（1）的一种或多种配体与铁盐或锰盐的反应在丙酮/水混合物中在温度 范围为0至50℃，为此目的，将式（1）的一种或多种配体在丙酮中的溶液或悬浮液与铁盐水溶液的金属盐溶液接触 r锰盐在发生反应的温度范围内。

    Method For Producing Bridged Manganese Complexes Of Triazacyclononane
    6.
    发明申请
    Method For Producing Bridged Manganese Complexes Of Triazacyclononane 有权
    生产三氮杂环壬烷锰配合物的方法

    公开(公告)号：US20120202990A1

    公开(公告)日：2012-08-09

    申请号：US13394968

    申请日：2010-09-10

    Applicant: Gerd Reinhardt ,  Michael Best ,  Christian Sidot

    Inventor： Gerd Reinhardt ,  Michael Best ,  Christian Sidot

    IPC: C07F13/00

    CPC classification number: C07F13/005 ,  B01J31/182 ,  B01J31/2208 ,  B01J2531/0216

    Abstract: The invention relates to a method for producing manganese complex compounds of the general formula (1), wherein M, X, L, z, Y and q are defined as in claim 1. The method is characterized by the following steps: a) reacting one or more bivalent metal salts with the ligand L in water as the solvent to form a coordination compound from the one or more bivalent metal salt and the ligand L, the one or more bivalent metal salts being selected from bivalent manganese salts and iron salts and at least one bivalent metal salt being a bivalent manganese salt, b) oxidizing the coordination compound of step a) with an oxidant while at the same time maintaining a pH of 11 to 14, to transform the metal M from the bivalent to the trivalent and/or tetravalent form, c) reducing the pH of the reaction mixture to a pH of 4 to 9 and removing any metal oxides or metal hydroxides of the metal M formed and d) adding, at a pH of 4 to 9, a salt of the formula MezYq, wherein Me represents an alkali metal ion, ammonium ion or an alkanol ammonium ion, and Y, z and q are defined as in formula (1).

    Abstract translation: 本发明涉及一种制备通式（1）的锰络合物的方法，其中M，X，L，Z，Y和q如权利要求1中所定义。该方法的特征在于以下步骤：a） 一种或多种二价金属盐与水中的配体L作为溶剂，以从一种或多种二价金属盐和配体L形成配位化合物，一种或多种二价金属盐选自二价锰盐和铁盐，以及 至少一种二价金属盐是二价锰盐，b）用氧化剂氧化步骤a）的配位化合物，同时保持pH为11至14，以将金属M从二价转化成三价和 /或四价形式，c）将反应混合物的pH降低至4至9的pH，并除去形成的金属M的任何金属氧化物或金属氢氧化物，以及d）在pH4至9的条件下，加入 式MezYq，其中Me表示碱金属离子，a 铵离子或烷醇铵离子，Y，Z和q如式（1）所定义。

    Racemoselective synthesis of rac-diorganosilylbis(2-methylbenzo[e]indeyl)zirconium compounds
    7.
    发明授权
    Racemoselective synthesis of rac-diorganosilylbis(2-methylbenzo[e]indeyl)zirconium compounds 失效
    外消旋 - 二有机甲硅烷基双（2-甲基苯并[e]茚满）锆化合物的外消旋选择性合成

    公开(公告)号：US07098354B2

    公开(公告)日：2006-08-29

    申请号：US10532511

    申请日：2003-10-22

    Applicant: Hans-Robert Damrau ,  Patrik Müller ,  Valerie Garcia ,  Christian Sidot ,  Christian Tellier ,  Jean-Francois Lelong

    Inventor： Hans-Robert Damrau ,  Patrik Müller ,  Valerie Garcia ,  Christian Sidot ,  Christian Tellier ,  Jean-Francois Lelong

    IPC: C07F17/00 ,  B01J31/00

    CPC classification number: C07F17/00 ,  C07F15/0073 ,  C08F10/00 ,  Y10S526/943 ,  C08F4/65927

    Abstract: The present invention relates to a specific process for the diastereoselective synthesis of rac-diorganosilylbis(2-methylbenzo[e]indenyl)zirconium compounds of the formula I, by reacting the silyl-bridged bisindenyl ligand with a dihalozirconium bis(3,5-di-tert-butylphenoxide)-base adduct to form the diorganosilylbis(2-methylbenzo[e]indenyl)zirconium bis(3,5-di-tert-butylphenoxide) and subsequently replacing the phenoxide groups by X using suitable replacement reagents to give the compound of the formula I; where the substituents X can be identical or different and are each F, Cl, Br, I or linear, cyclic or branched C1-10-alkyl; and the substituents R can be identical or different and are each linear, cyclic or branched C1-10-alkyl or C6-10-aryl; and also to the use of these compounds as catalysts.

    Abstract translation: 本发明涉及通过使甲硅烷基桥连的双茚基配体与二卤代双（3,5-二（二苯基）环己基）二卤代锆反应来非对映选择性合成式I的外消旋二有机甲硅烷基双（2-甲基苯并[e]茚基） - 叔丁基苯酚） - 基加成物形成二有机甲硅烷基双（2-甲基苯并[e]茚基）双（3,5-二叔丁基苯氧基）锆，随后用合适的替代试剂将X代替苯酚基，得到化合物 的式I; 其中取代基X可以相同或不同，并且各自为F，Cl，Br，I或直链，环状或支链C 1-10 - 烷基; 并且取代基R可以相同或不同，并且各自是直链，环状或支链C 1-10 - 烷基或C 6-10 - 芳基; 以及这些化合物作为催化剂的使用。

    Industrial process for the continuous preparation of sodium orthohydroxymandelate
    8.
    发明授权
    Industrial process for the continuous preparation of sodium orthohydroxymandelate 失效
    连续制备邻羟基扁桃酸钠的工业过程

    公开(公告)号：US5914429A

    公开(公告)日：1999-06-22

    申请号：US33435

    申请日：1998-03-02

    Applicant: Christian Sidot

    Inventor： Christian Sidot

    IPC: B01J31/26 ,  C07B61/00 ,  C07C51/367 ,  C07C59/48

    CPC classification number: C07C51/367 ,  Y02P20/582

    Abstract: In an industrial process for the manufacture of sodium orthohydroxymandelate by condensation of phenol in an inert atmosphere with glyoxylic acid in aqueous solution, in the presence of a tertiary amine and of catalytic quantities of a trivalent metal cation at a temperature below 100.degree. C., carried out continuously in at least two reactors (R1 . . . Rn) installed in series, the first being supplied by a first tank C1 containing the glyoxylic acid and the trivalent metal cations, and a second tank C2 containing the phenol and the tertiary amine, the reaction medium obtained at the outlet of the last of the at least two reactors and consisting of an aqueous phase and an organic phase is transferred into the first of two mixer-decanters (MD1 and MD2) installed in series, the aqueous phase of the first mixer-decanter MD1 is recovered in order to extract the expected sodium orthohydroxymandelate from it, while the organic phase that has come from MD1 is transferred into the second mixer-decanter MD2 and washed with water, and the organic phase of the second mixer-decanter MD2 is transferred to the second tank (C2).

    Abstract translation: 在惰性气氛中苯酚与乙醛酸在水溶液中的存在下，在叔胺和催化量的三价金属阳离子的存在下，在低于100℃的温度下，制备邻羟基扁桃酸钠的工业方法中， 在至少两个串联安装的反应器（R1 ... Rn）中连续进行，首先由含有乙醛酸和三价金属阳离子的第一罐C1供应，以及含有苯酚和叔胺的第二罐C2 在最后的至少两个反应器的出口处获得的由水相和有机相组成的反应介质被转移到串联安装的两个混合器 - 滗析器（MD1和MD2）中的第一个中，水相 回收第一混合器 - 滗析器MD1以从其中提取预期的邻羟基扁桃酸钠，而来自MD1的有机相转移到第二混合器-d ecanter MD2并用水洗涤，第二混合器 - 倾析器MD2的有机相转移到第二罐（C2）。

    Process for Recycling Cyclopentadienyl Derivatives and Preparing Metallocenes From Recycled, Substituted Cyclopentadienyl Derivatives
    9.
    发明申请
    Process for Recycling Cyclopentadienyl Derivatives and Preparing Metallocenes From Recycled, Substituted Cyclopentadienyl Derivatives 有权
    回收环戊二烯基衍生物的方法和从再循环的取代的环戊二烯基衍生物制备金属茂

    公开(公告)号：US20100274035A1

    公开(公告)日：2010-10-28

    申请号：US12086711

    申请日：2006-12-19

    Applicant: Patrik Müller ,  Robert L. Jones ,  Reynald Chevalier ,  Christian Sidot ,  Valerie Garcia

    Inventor： Patrik Müller ,  Robert L. Jones ,  Reynald Chevalier ,  Christian Sidot ,  Valerie Garcia

    IPC: C07F17/00 ,  C07C7/12

    CPC classification number: C07F17/00 ,  C07C7/12 ,  C07F7/0832 ,  C07C13/465

    Abstract: The present invention relates to a process for recycling cyclopentadienyl derivatives of the formulae (I) and (I′), a process for preparing metallocenes of the formula (III) from cyclopentadienyl derivatives of the formulae (I) and (I′) or from bridged biscyclopentadienyl derivatives of the formula (II), in which the cyclopentadienyl derivatives of the formulae (I), (I′) or (II) which are used have been at least partly recovered and purified by means of liquid-solid chromatography, and the use of liquid-solid chromatography for purifying substituted, recovered cyclopentadienyl derivatives of the formulae (I), (I′) or (II).

    Abstract translation: 本发明涉及用于回收式（I）和（I'）的环戊二烯基衍生物的方法，由式（I）和（I'）的环戊二烯基衍生物制备式（III）的金属茂的方法或 式（II）的桥连双环戊二烯基衍生物，其中使用的式（I），（I'）或（II）的环戊二烯基衍生物已经通过液固色谱至少部分回收和纯化，以及 使用液 - 固色谱来纯化式（I），（I'）或（II）的取代的回收的环戊二烯基衍生物。

    Process for the racemoselective preparation of ansa-metallocenes
    10.
    发明授权
    Process for the racemoselective preparation of ansa-metallocenes 有权

    公开(公告)号：US07671223B2

    公开(公告)日：2010-03-02

    申请号：US11579526

    申请日：2005-05-04

    Applicant: Valerie Garcia ,  Patrik Müller ,  Christian Sidot ,  Christian Tellier ,  Ludovic Delancray ,  Reynald Chevalier

    Inventor： Valerie Garcia ,  Patrik Müller ,  Christian Sidot ,  Christian Tellier ,  Ludovic Delancray ,  Reynald Chevalier

    IPC: C07F17/00 ,  C07F7/00

    CPC classification number: C07F17/00

    Abstract: The present invention relates to a process for the racemoselective preparation of ansa-metallocene complexes of the formula (I) which comprises reacting a ligand starting compound of the formula (II) with a transition metal compound of the formula (III) (LB)yM1(NR3R4)Xx-1  (III) where R1, R1′ are identical or different and are each hydrogen or an organic radical having from 1 to 40 carbon atoms, R2, R2′ are identical or different and are each hydrogen or an organic radical having from 1 to 40 carbon atoms, R3 is an organic radical having from 1 to 40 carbon atoms, R4 is hydrogen or an organic radical having from 1 to 40 carbon atoms, T, T′ are identical or different and are each a divalent organic group which has from 1 to 40 carbon atoms and together with the cyclopentadienyl ring forms at least one further saturated or unsaturated, substituted or unsubstituted ring system which has a ring size of from 5 to 12 atoms, where T and T′ may contain the heteroatoms Si, Ge, N, P, As, Sb, O, S, Se or Te within the ring system fused to the cyclopentadienyl ring, A is a bridge consisting of a divalent atom or a divalent group, M1 is an element of group 3, 4, 5 or 6 of the Periodic Table of the Elements or the lanthanides, the radicals X are identical or different and are each an organic or inorganic radical which can be substituted by a cyclopentadienyl anion, x is a natural number from 3 to 6, M2 is an alkali metal, an alkaline earth metal or a magnesium monohalide fragment, p is 1 in the case of doubly positively charged metal ions or is 2 in the case of singly positively charged metal ions or metal ion fragments, LB is an uncharged Lewis-base ligand and y is a natural number from 0 to 6, and also a further process for the racemoselective preparation of ansa-metallocene complexes of the formula (IV) starting from the metallocene complexes of the formula (I) prepared by the first process, the use of transition metal compounds of the formula (III) for preparing metallocenes and also specific transition metal compounds of the formula (III).

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