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公开(公告)号：US6129863A
公开(公告)日：2000-10-10
申请号：US216463
申请日：1998-12-18
申请人： John Y. Lee , David W. Owens , Charles R. Everly , Ronny W. Lin , John M. Power , Steven P. Diefenbach , Niomi L. Krzystowczyk
发明人： John Y. Lee , David W. Owens , Charles R. Everly , Ronny W. Lin , John M. Power , Steven P. Diefenbach , Niomi L. Krzystowczyk
摘要： Perfluoroaryl Grignard reagents are produced from a hydrocarbyl Grignard reagent and polyhaloaromatic compounds via separate additions of different polyhaloaromatic compounds, such that the conversion of hydrocarbyl Grignard reagent to the desired perfluoroaryl Grignard reagent is essentially complete, and thus the reaction product is free or essentially free of agents that may negatively affect subsequent reactions. The perfluoroaryl Grignard reagents may be further reacted with boron trihalides in order to obtain tris(perfluoroaryl)boranes or tetrakis(perfluoroaryl)borates.
摘要翻译： 全氟芳基格氏试剂由烃基格利雅试剂和多卤代芳族化合物通过分别添加不同的多卤芳族化合物制备，使得烃基格氏试剂转化为所需的全氟芳基格氏试剂基本上完全，因此反应产物是游离的或基本上不含 可能会对后续反应产生负面影响的药剂。 可以将全氟芳基格氏试剂进一步与三卤化硼反应，以获得三（全氟芳基）硼烷或四（全氟芳基）硼酸盐。
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公开(公告)号：US5959151A
公开(公告)日：1999-09-28
申请号：US58408
申请日：1998-04-09
申请人： John Y. Lee , Steven P. Diefenbach , John M. Power , Ronny W. Lin
发明人： John Y. Lee , Steven P. Diefenbach , John M. Power , Ronny W. Lin
IPC分类号： C07F5/02
CPC分类号： C07F5/027
摘要： One aspect of the invention is a process for purifying a pentafluorophenyl boron compound from a crude mixture comprised of the pentafluorophenyl boron compound and impurities, the impurities at least comprised of an ether and water, the process comprising: (a) mixing the crude mixture with an azeotropic organic solvent which (i) is capable of azeotrope formation with the water and (ii) has a boiling point above the boiling point of the ether; (b) distilling the resulting solution to remove at least a portion of the impurities; and (c) cooling the distilled solution so that a precipitate comprised of the pentafluorophenyl boron compound is formed. Processes are also described for producing pentafluorophenyl boron compounds which are particularly pure, dry and fine.
摘要翻译： 本发明的一个方面是从由五氟苯基硼化合物和杂质构成的粗混合物中纯化五氟苯基硼化合物的方法，所述杂质至少由醚和水组成，所述方法包括：（a）将粗混合物与 （i）能够与水共沸形成的共沸有机溶剂，和（ii）沸点高于乙醚的沸点; （b）蒸馏所得溶液以除去至少一部分杂质; 和（c）冷却蒸馏溶液使得形成由五氟苯基硼化合物构成的沉淀物。 还描述了制备特别纯的，干燥的和细的五氟苯基硼化合物的方法。
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公开(公告)号：US06248265B1
公开(公告)日：2001-06-19
申请号：US09596146
申请日：2000-06-16
申请人： John Y. Lee , David W. Owens , Charles R. Everly , Ronny W. Lin , John M. Power , Steven P. Diefenbach , Niomi L. Krzystowczyk
发明人： John Y. Lee , David W. Owens , Charles R. Everly , Ronny W. Lin , John M. Power , Steven P. Diefenbach , Niomi L. Krzystowczyk
IPC分类号： C07F302
摘要： Fluoroaryl Grignard reagents are produced from a hydrocarbyl Grignard reagent and fluoroaromatic compounds via separate additions of different fluoroaromatic compounds, such that the conversion of hydrocarbyl Grignard reagent to the desired fluoroaryl Grignard reagent is essentially complete, and thus the reaction product is free or essentially free of agents that may negatively affect subsequent reactions. The fluoroaryl Grignard reagents may be further reacted with boron trihalides in order to obtain tris(fluoroaryl)boranes or tetrakis(fluoroaryl)borates.
摘要翻译： 氟芳基格氏试剂由烃基格氏试剂和氟代芳族化合物通过分别添加不同的氟代芳族化合物制备，使得烃基格氏试剂转化为所需的氟代芳基格氏试剂基本上完全，因此反应产物是游离的或基本上不含 可能会对后续反应产生负面影响的药剂。 氟化芳基格氏试剂可以进一步与三卤化硼反应，以获得三（氟化芳基）硼烷或四（氟化芳基）硼酸盐。
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公开(公告)号：US5302733A
公开(公告)日：1994-04-12
申请号：US860339
申请日：1992-03-30
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。
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公开(公告)号：US5936108A
公开(公告)日：1999-08-10
申请号：US998105
申请日：1997-12-24
申请人： Ronny W. Lin , Bruce C. Berris , John M. Power , Troy E. DeSoto , John F. Balhoff , Jamie R. Strickler
发明人： Ronny W. Lin , Bruce C. Berris , John M. Power , Troy E. DeSoto , John F. Balhoff , Jamie R. Strickler
CPC分类号： C07F17/00 , Y10S526/943
摘要： A metallocene having one or two hydrocarbyl groups bonded to a Group 4 metal are produced from a crude impure pasty or non-wet mixture containing at least 50% by weight of a metallocene having two halogen atoms bonded to a Group 4 metal atom, by (a) mixing liquid aromatic hydrocarbon with the crude impure pasty or non-wet mixture; (b) mixing a solution of an organolithium compound in a suitable anhydrous ether or paraffinic hydrocarbon solvent or a mixture thereof, with the mixture from (a) and agitating the resulting mixture so that lithium halide solids are formed; and (c) separating the solids and recovering the resultant liquid portion which is mainly a solution of the metallocene having one or two hydrocarbyl groups bonded to a Group 4 metal. Additional optional steps include (d) replacing the original solvent from the solution from (c) with a liquid paraffinic hydrocarbon diluent to form a slurry of product solids; and (e) recovering the product metallocene solids. Preferred organolithium compounds have the formula, RLI.nLiX, where R is tert-alkyl, aryl, alkaryl, benzyl, or alkyl-substituted benzyl, or most preferably, methyl, and X is Br or I.
摘要翻译： 具有与第4族金属键合的具有一个或两个烃基的茂金属由粗制不纯的糊状或非湿混合物制备，所述混合物含有至少50重量％的具有两个与第4族金属原子键合的卤素原子的茂金属，通过（ a）将液体芳烃与粗不纯的糊状或非湿混合物混合; （b）将有机锂化合物在合适的无水醚溶剂或链烷烃溶剂或其混合物中的溶液与来自（a）的混合物混合并搅拌所得混合物使得形成卤化锂固体; 和（c）分离固体并回收所得液体部分，其主要是具有键合到第4族金属上的一个或两个烃基的茂金属溶液。 另外的任选步骤包括（d）将来自（c）的溶液中的原始溶剂用液体石蜡烃稀释剂代替以形成产物固体的浆液; 和（e）回收产物茂金属固体。 优选的有机锂化合物具有下式：RLI.nLiX，其中R是叔烷基，芳基，烷芳基，苄基或烷基取代的苄基，或最优选甲基，X是Br或I.
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公开(公告)号：US5883278A
公开(公告)日：1999-03-16
申请号：US945653
申请日：1997-01-20
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 chelate diamine adduct of a transition, lanthanide, or actinide metal halide in an organic solvent medium so as to produce said chiral metallocene.
摘要翻译： PCT No.PCT / US96 / 05089第 371日期1998年1月20日 102（e）日期1998年1月20日PCT提交1996年4月12日PCT公布。 出版物WO96 / 34002 日期1996年10月31日通过使含有不对称双（环戊二烯基）部分的配体的盐与过渡金属镧系元素或锕系金属卤化物的螯合二胺加合物在有机溶剂介质中反应制备手性茂金属，以便产生所述手性茂金属 。
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公开(公告)号：US5847175A
公开(公告)日：1998-12-08
申请号：US833110
申请日：1997-04-04
申请人： Jamie R. Strickler , John M. Power
发明人： Jamie R. Strickler , John M. Power
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 chelate diamine 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： 通过使不对称双（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螯合二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。
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公开(公告)号：US5679814A
公开(公告)日：1997-10-21
申请号：US570031
申请日：1995-12-11
申请人： Jamie R. Strickler , John M. Power
发明人： Jamie R. Strickler , John M. Power
CPC分类号： C07F17/00
摘要： Metallocenes, such as silicon bridged ansa-metallocenes, are purified by heating a slurry of the metallocene at elevated temperature in an aprotic, polar solvent so as to extract impurities from the metallocene into the solvent and then separating the impurity containing solvent from the metallocene.
摘要翻译： 通过在非质子极性溶剂中在升高的温度下加热茂金属的浆料以将杂质从金属茂中提取到溶剂中，然后从茂金属中分离出含杂质的溶剂，从而对金属茂如硅桥连金属茂进行纯化。
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公开(公告)号：US5556997A
公开(公告)日：1996-09-17
申请号：US427505
申请日：1995-04-24
申请人： Jamie R. Strickler , John M. Power
发明人： Jamie R. Strickler , John M. Power
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 chelate diamine adduct of a transition, lanthanide, or actinide metal halide in an organic solvent medium so as to produce said chiral metallocene.
摘要翻译： 通过使含有不对称双（环戊二烯基）部分的配体的盐与过渡金属镧系元素或锕系金属卤化物的螯合二胺加成物在有机溶剂介质中反应以制备手性茂金属来制备手性金属茂。
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公开(公告)号：US5359105A
公开(公告)日：1994-10-25
申请号：US144463
申请日：1993-11-01
申请人： Jamie R. Strickler , John M. Power
发明人： Jamie R. Strickler , John M. Power
摘要： Cyclopentadienyl derivatives are deprotonated by a process whereby the cyclopentadienyl derivatives are reacted with a Grignard reagent in an inert solvent which contains from about 0.5 to 1.5 equivalents per equivalent of cyclopentadienyl derivative of a cyclic ether or an acyclic polyether, so as to form a dianionic salt of said cyclopentadienyl derivative.
摘要翻译： 环戊二烯基衍生物通过使环戊二烯基衍生物与格氏试剂在含有约0.5至1.5当量/当量环醚或无环聚醚的环戊二烯基衍生物的惰性溶剂中反应的方法去质子化，以形成二阴离子盐 的所述环戊二烯基衍生物。
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