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    PROCESS FOR PRODUCING N-HALOGENATED ORGANIC COMPOUNDS
    1.
    发明申请
    PROCESS FOR PRODUCING N-HALOGENATED ORGANIC COMPOUNDS 审中-公开
    生产N-卤代有机化合物的方法

    公开(公告)号：WO2006023167A3

    公开(公告)日：2006-04-13

    申请号：PCT/US2005025080

    申请日：2005-07-12

    Applicant: ALBEMARLE CORP ,  PETERS BRUCE C ,  SPIELMAN EDGE E JR ,  THOMAS DUSTIN H ,  ELNAGAR HASSAN Y

    Inventor： PETERS BRUCE C ,  SPIELMAN EDGE E JR ,  THOMAS DUSTIN H ,  ELNAGAR HASSAN Y

    IPC: C07D233/72 ,  C07D233/82 ,  C07D233/74

    CPC classification number: C07D233/82

    Abstract: The process enables highly effective N-halogenation of a compound having one or more halogenatable amido or imido functional groups in the molecule. The process involves, for example, concurrently feeding into a reactor (i) water, inorganic base, and the compound to be N-halogenated, e.g., a hydantoin, and a feed of (ii) a brominating agent and/or a chlorinating agent. The proportions of these feeds are such that the pH is kept at 5 or below or within a specified range e.g., 5.5-8.5 and one or more of the amido or imido nitrogen atoms is substituted by a bromine or chlorine atom. A feature of the process is that it can be conducted at elevated temperatures as high as about 90 ° C without appreciable thermal decomposition of reactants or product. The resultant product continuously precipitates in high yield and purity. Moreover, products can be produced that are very pale yellow to almost pure white in appearance. Further, the process has been found capable of producing 1,3-dibromo-5,5-dimethylhydantoin with far larger particle sizes than previously produced on a commercial basis.

    Abstract translation: 该方法能够对分子中具有一个或多个可卤代酰胺或亚氨基官能团的化合物进行高度有效的N-卤化。 该方法包括例如同时将反应器（i）水，无机碱和待卤化的化合物（例如乙内酰脲）和（ii）溴化剂和/或氯化剂 。 这些进料的比例是使得pH保持在5或低于或在特定范围内，例如5.5-8.5，并且一个或多个酰氨基或亚氨基氮原子被溴或氯原子取代。 该方法的一个特征是它可以在高达约90°C的高温下进行而没有明显的反应物或产物的热分解。 所得产物以高收率和高纯度连续沉淀。 此外，产品可以生产非常浅黄色至外观几乎纯白色。 此外，已经发现该方法能够生产具有比之前以商业方式生产的更大的粒径的1,3-二溴-5,5-二甲基乙内酰脲。

    PRODUCTION OF BRIDGED METALLOCENE COMPLEXES AND INTERMEDIATES THEREFOR
    2.
    发明申请
    PRODUCTION OF BRIDGED METALLOCENE COMPLEXES AND INTERMEDIATES THEREFOR 审中-公开
    桥联金属络合物的生产及其中间体

    公开(公告)号：WO9749712A3

    公开(公告)日：1998-02-26

    申请号：PCT/US9710684

    申请日：1997-06-20

    Applicant: ALBEMARLE CORP

    Inventor： AO MENG-SHENG ,  ELNAGAR HASSAN Y ,  MALCOLM ARCELIO J ,  STRICKLER JAMIE R ,  LIN RONNY W ,  BALHOFF JOHN F

    IPC: C07F7/22 ,  C07F7/30 ,  C07F17/00 ,  C07C5/00 ,  C07F7/07 ,  C08F10/00

    CPC classification number: C07F7/0827 ,  C07F7/2212 ,  C07F7/30 ,  C07F17/00

    Abstract: Bridged metallocene compounds are produced by a process of promising commercial utility for plant-sized operations. One of the key steps of the process involves converting a deprotonated silicon-, germanium- or tin-containing ligand into the metallocene. Preferably, and in accordance with an embodiment of the invention, this is accomplished to great advantage by adding a diamine adduct of a Group IV, V, or VI metal tetrahalide to a solution or slurry formed from a deprotonated silicon-, germanium- or tin-containing ligand and an organic liquid medium so as to form a metallocene. The overall process of the invention involves the direct conversion of benzoindanones to benzoindanols which, without isolation, are converted to benzoindenes. Thereupon the benzoindenes are bridged by deprotonating the benzoindenes with a strong base such as butyllithium and reacting the resultant deprotonated product with a suitable silicon-, germanium- or tin-containing bridging reactant such as dichlorodimethylsilane. The resultant bridged product is deprotonated with a strong base such as butyllithium and reacted with a suitable Group IV, V, or VI metal-containing reactant such as ZrCl4 to provide a silicon-, germanium- or tin-bridged Group IV, V, or VI metal complex, such as a dihydrocarbylsilyl-bridged zirconocene complex.

    Abstract translation: 桥接的茂金属化合物是通过有希望的用于植物大小的操作的商业应用的方法生产的。 该方法的关键步骤之一涉及将去质子化的含硅或锗的配体转化为茂金属。 优选地，并且根据本发明的一个实施方案，这通过将IV，V或VI族金属四卤化物的二胺加合物加入到由去质子化的硅，锗或锡形成的溶液或浆料中来实现， 的配体和有机液体介质，以形成茂金属。 本发明的总体方法涉及将苯并二氢醌直接转化为苯并二醇，其不经分离转化为苯并茚基。 因此，苯并茚基通过用强碱如丁基锂对苯并茚进行去质子化来桥接，并使得到的去质子化产物与合适的含硅，锗或锡的桥连反应物如二氯二甲基硅烷反应。 所得的桥连产物用强碱如丁基锂去质子化并与合适的含IV，V或VI族金属的反应物如ZrCl 4反应以提供硅，锗或锡桥连的IV族V，或 VI金属络合物，例如二烃基甲硅烷基桥接的茂锆复合物。

    PROCESS FOR PRODUCING N-HALOGENATED ORGANIC COMPOUNDS
    4.
    发明申请
    PROCESS FOR PRODUCING N-HALOGENATED ORGANIC COMPOUNDS 审中-公开
    生产N-有机有机化合物的方法

    公开(公告)号：WO0153270A3

    公开(公告)日：2002-02-14

    申请号：PCT/US0101544

    申请日：2001-01-17

    Applicant: ALBEMARLE CORP

    Inventor： ELNAGAR HASSAN Y ,  PETERS BRUCE C ,  SPIELMAN EDGAR E JR ,  THOMAS DUSTIN H

    IPC: C07D233/72 ,  C07D233/74 ,  C07D233/82 ,  C07D251/36

    CPC classification number: C07D233/82

    Abstract: The process enables highly effective N-halogenation of a compound having one or more halogenatable amido or imido functional groups in the molecule. The process involves, for example, concurrently feeding into a reactor (i) water, inorganic base, and the compound to be N-halogenated, e.g., a hydantoin, and a feed of (ii) a brominating agent and/or a chlorinating agent. The proportions of these feeds are such that the pH is kept within the range of ca. 5.5-8.5 (preferably 6.5-8.5, and most preferably 6.8-7.2) and one or more of the amido or imido nitrogen atoms is substituted by a bromine or chlorine atom. A feature of the processs is that it can be conducted at elevated temperatures as high as about 90 DEG C without appreciable thermal decomposition of reactants or product. The resultant product continuously precipitates in high yield and purity. Moreover, products can be produced that are very pale yellow to almost pure white in appearance. Further, the process has been found capable of producing 1,3-dibromo-5,5-dimethylhydantoin with far larger particle sizes than previously produced on a commercial basis.

    Abstract translation: 该方法能够在分子中具有一个或多个可卤化酰氨基或亚氨基官能团的化合物的高效N-卤化。 该方法包括例如同时加入反应器（i）水，无机碱和待卤化的化合物，例如乙内酰脲，和（ii）溴化剂和/或氯化剂的进料 。 这些进料的比例使得pH保持在约 5.5-8.5（优选6.5-8.5，最优选6.8-7.2），一个或多个酰胺基或亚氨基氮原子被溴或氯原子取代。 该方法的特征在于它可以在高达约90℃的高温下进行，而没有明显的反应物或产物的热分解。 所得产物以高产率和纯度连续沉淀。 此外，可以生产非常浅黄色至几乎纯白色的产品。 此外，已经发现该方法能够生产出比以前在商业上生产的粒度大得多的1,3-二溴-5,5-二甲基乙内酰脲。

    1,3-DIBROMO-5,5-DIMETHYLHYDANTOIN OF ENHANCED PROPERTIES
    7.
    发明申请
    1,3-DIBROMO-5,5-DIMETHYLHYDANTOIN OF ENHANCED PROPERTIES 审中-公开
    1,3-DIBROMO-5,5-DIMETHYLHYDANTOIN的增强性能

    公开(公告)号：WO0152656A3

    公开(公告)日：2002-03-21

    申请号：PCT/US0101585

    申请日：2001-01-17

    Applicant: ALBEMARLE CORP

    Inventor： ELNAGAR HASSAN Y ,  HOWARTH JONATHAN N ,  PETERS BRUCE C ,  SPIELMAN EDGAR E JR ,  THOMAS DUSTIN H

    IPC: C07D233/54 ,  A01N25/12 ,  A01N43/50 ,  A01N59/00 ,  B01J2/22 ,  C07D233/82

    CPC classification number: C07D233/82 ,  A01N59/00 ,  Y10S514/951 ,  A01N25/34 ,  A01N25/12 ,  A01N2300/00

    Abstract: Among the enhanced properties of the 1,3-dibromo-5,5-dimethylhydantoins described are their larger average particle sizes, their compactibility even though devoid of a binder, their excellent free-flowing and low-dust properties, and their more appealing aesthetic qualities, as compared to previously known 1,3-dibromo-5,5-dimethylhydantoins. These novel 1,3-dibromo-5,5-dimethyl-hydantoins can be produced, for example, by concurrently feeding (i) an aqueous solution or slurry formed from an inorganic base and 5,5-dimethylhydantoin, and (ii) a brominating agent, in proportions such that each nitrogen atom is substituted by a bromine atom, thereby forming product which precipitates in an aqueous reaction mixture. The pH of the reaction mixture is maintained in the range of 5.5 to 8.5.

    Abstract translation: 所描述的1,3-二溴-5,5-二甲基乙内酰脲的增强性能是它们更大的平均粒度，即使没有粘合剂，它们的优异的自由流动性和低灰尘性质，以及它们更具吸引力的美学 质量，与以前已知的1,3-二溴-5,5-二甲基乙内酰脲相比。 这些新的1,3-二溴-5,5-二甲基 - 乙内酰脲可以例如通过同时进料（i）由无机碱和5,5-二甲基乙内酰脲形成的水溶液或浆料来制备，和（ii） 溴化剂，其比例使得每个氮原子被溴原子取代，从而形成在水性反应混合物中沉淀的产物。 反应混合物的pH值保持在5.5至8.5的范围内。

    BENZYLIC HALOGENATION OF ALKYLBENZOIC ACID ESTERS
    8.
    发明申请
    BENZYLIC HALOGENATION OF ALKYLBENZOIC ACID ESTERS 审中-公开
    苄基苯甲酸酯的苯甲酸酯化

    公开(公告)号：WO0053564A3

    公开(公告)日：2000-12-28

    申请号：PCT/US0006190

    申请日：2000-03-08

    Applicant: ALBEMARLE CORP

    Inventor： ELNAGAR HASSAN Y

    IPC: C07C67/307 ,  C07C69/76 ,  C07C69/78

    CPC classification number: C07C67/307 ,  C07C69/76

    Abstract: Direct preparation of benzylically halogenated alkylbenzoic acid ester from an alkylbenzoic acid ester in which the alkyl group is a primary or secondary alkyl group is carried out. The ester group of the starting ester (i) is devoid of non-aromatic unsaturation and (ii) if an aromatic group, is devoid of ring substitution that would undergo benzylic halogenation. The process comprises slowly feeding halogen continuously and/or intermittently to an agitated solution of the alkylbenzoic acid ester in a liquid halogen-containing solvent maintained at a thermal halogenation temperature such that when the alkyl group of the alkylbenzoic acid ester is a primary alkyl group and monohalogenation is desired, the total amount of halogen fed does not exceed about 0.8 mole of halogen per mole of alkylbenzoic acid ester. If the alkylbenzoic acid ester is a toluic acid ester and dihalogenation is desired, the amount of halogen fed is over (1) mole but no more than about 1.8 moles per mole of the toluic acid ester. Ester cleavage is minimized and other advantages are made possible.

    Abstract translation: 从其中烷基是伯或仲烷基的烷基苯甲酸酯直接制备苄基卤代烷基苯甲酸酯。 起始酯（i）的酯基没有非芳族不饱和键，和（ii）如果芳族基团没有将进行苄基卤化的环取代。 该方法包括将卤代烷连续地和/或间歇地慢慢地加入烷基苯甲酸酯的搅拌溶液中，该溶液保持在热卤化温度下，使得当烷基苯甲酸酯的烷基是伯烷基和 需要单卤代化，每摩尔烷基苯甲酸酯的卤素供体总量不超过约0.8摩尔的卤素。 如果烷基苯甲酸酯是甲苯甲酸酯并且需要二卤代，则每摩尔甲苯甲酸酯的卤素加入量超过（1）摩尔但不超过约1.8摩尔。 酯切割最小化，其他优点成为可能。

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