Process for transhalogenating a halophosphorous compound with anhydrous
hydrogen fluoride
    22.
    发明授权
    Process for transhalogenating a halophosphorous compound with anhydrous hydrogen fluoride 失效
    用无水氟化氢将卤代磷化合物转化成卤素的方法

    公开(公告)号:US5049691A

    公开(公告)日:1991-09-17

    申请号:US487787

    申请日:1990-03-05

    IPC分类号: C07F9/146 C07F9/6574

    CPC分类号: C07F9/146 C07F9/65744

    摘要: Phosphorus compounds having at least one chlorine, bromine or iodine bonded directly to phosphorus are transhalogenated with fluorine by reaction with anhydrous hydrogen fluoride in an inert solvent, e.g., xylene, methylene chloride, in a manner such that said anhydrous hydrogen fluoride is added to said phosphorus compound at a rate such that said anhydrous hydrogen fluoride reacts with said phosphorus compound without the accumulation of an amount of unreacted anhydrous hydrogen fluoride which is sufficient to cause substantial decomposition of the desired fluorophosphorus product.

    摘要翻译: 具有至少一个直接与磷结合的氯,溴或碘的磷化合物通过与惰性溶剂(例如二甲苯,二氯甲烷)中的无水氟化氢反应,与氟反式氟化,使得所述无水氟化氢加入所述 磷化合物,其使得所述无水氟化氢与所述磷化合物反应而不累积一定量的未反应的无水氟化氢,其足以引起所需氟磷产物的显着分解。

    Process for making decabromodiphenyl oxide
    23.
    发明授权
    Process for making decabromodiphenyl oxide 失效
    十溴二苯醚的制备方法

    公开(公告)号:US4778933A

    公开(公告)日:1988-10-18

    申请号:US73704

    申请日:1987-07-15

    CPC分类号: C07C41/22 C07C41/42

    摘要: The process comprises: (a) initiating a feed of molten diphenyl oxide to a substantially anhydrous mixture of methylene dibromide solvent, elemental bromine (Br.sub.2) and an aluminum trihalide catalyst at a temperature between about 10.degree. and about 30.degree. C.; (b) heating the reaction mixture to about 50.degree.-60.degree. C., and while maintaining the temperature at about 50.degree.-60.degree. C., continuing the feed of molten diphenyl oxide until the total amount fed is equivalent to (i) about 0.064 to about 0.077 mole per mole of elemental bromine (Br.sub.2) employed in the reaction, and (ii) about 0.2 to about 10 parts by weight per part by weight of methylene dibromide employed in the reaction; (c) steam distilling the methylene dibromide solvent and the residual bromine from the reaction mixture; (d) recovering decabromodiphenyl oxide from the distilland; and (e) drying the methylene dibromide and bromine distillate to render them suitable for reuse in the process.

    Enhanced synthesis of racemic metallocenes
    24.
    发明授权
    Enhanced synthesis of racemic metallocenes 有权
    增强外消旋金属茂合成

    公开(公告)号:US06252098B1

    公开(公告)日:2001-06-26

    申请号:US09586818

    申请日:2000-06-05

    IPC分类号: C07F1700

    CPC分类号: C07F17/00 Y10S526/943

    摘要: Chiral metallocenes are prepared by reacting a salt of an asymmetric bis(cyclopentadienyl)-moiety-containing ligand with a tertiary heteroaromiatic amine adduct of a transition, lanthanide, or actinide metal halide in an organic solvent or diluent so as to produce said chiral metallocene.

    摘要翻译: 通过将不对称双(环戊二烯基) - 含有配体的盐与过渡金属镧系元素或锕系金属卤化物的第三异构异构胺加成物在有机溶剂或稀释剂中反应以制备手性茂金属来制备手性金属茂。

    Process for transhalogenating a halophosphorus compound with fluoride
    26.
    发明授权
    Process for transhalogenating a halophosphorus compound with fluoride 失效
    用氟化物将卤代磷化合物氟化的方法

    公开(公告)号:US5136075A

    公开(公告)日:1992-08-04

    申请号:US723594

    申请日:1991-07-01

    IPC分类号: C07F9/146 C07F9/6574

    CPC分类号: C07F9/146 C07F9/65744

    摘要: Phosphorus compounds having at least one chlorine, bromine or iodine bonded directly to phosphorus are transhalogenated with fluorine by reaction with anhydrous hydrogen fluoride in an inert solvent, e.g., xylene, methylene chloride, in a manner such that said anhydrous hydrogen fluoride is added to said phosphorus compound at a rate such that said anhydrous hydrogen fluoride reacts with said phosphorus compound without the accumulation of an amount of unreacted anhydrous hydrogen fluoride which is sufficient to cause substantial decomposition of the desired fluorophosphorus product. A catalytic amount of a pyridine-type compound may optionally included in the reaction.

    摘要翻译: 具有至少一个直接与磷结合的氯,溴或碘的磷化合物通过与惰性溶剂(例如二甲苯,二氯甲烷)中的无水氟化氢反应,与氟反式氟化,使得所述无水氟化氢加入所述 磷化合物,其使得所述无水氟化氢与所述磷化合物反应而不累积一定量的未反应的无水氟化氢,其足以引起所需氟磷产物的显着分解。 催化量的吡啶型化合物可以任选地包括在反应中。

    Production of bridged metallocene complexes and intermediates therefor
    27.
    发明授权
    Production of bridged metallocene complexes and intermediates therefor 失效
    制备桥连金属茂配合物及其中间体

    公开(公告)号:US5861522A

    公开(公告)日:1999-01-19

    申请号:US853698

    申请日:1997-05-08

    摘要: 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 ZrCl.sub.4 to provide a silicon-, germanium- or tin-bridged Group IV, V, or VI metal complex, such as a dihydrocarbylsilyl-bridged zirconocene complex.

    摘要翻译: 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。

    Preparation of metallocenes
    28.
    发明授权
    Preparation of metallocenes 失效
    金属茂的制备

    公开(公告)号:US5302733A

    公开(公告)日:1994-04-12

    申请号:US860339

    申请日:1992-03-30

    IPC分类号: C07F17/00 C07F7/28

    CPC分类号: C07F17/00

    摘要: A racemic mixture of a chiral, silicon bridged transition metal metallocene, which is substantially free of meso isomer, is precipitated directly from a reaction mixture as it is formed by reacting an organic solvent solution of an alkali metal salt of a silicon bridged ligand with a transition metal tetrahalide-ether complex.

    摘要翻译: 基本上不含内消旋异构体的手性,硅桥连的过渡金属茂金属的外消旋混合物直接从反应混合物中沉淀,因为它是通过使硅桥联配体的碱金属盐的有机溶剂溶液与 过渡金属四卤化物 - 醚络合物。