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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：US5883296A
公开(公告)日：1999-03-16
申请号：US801051
申请日：1997-02-14
申请人： John M. Power , Bruce C. Berris , David A. Caillet
发明人： John M. Power , Bruce C. Berris , David A. Caillet
CPC分类号： C07F9/06 , C07C17/208 , C07F9/062
摘要： A mixture is made from (i) a tris(dihydrocarbylamino) phosphoroamidite and/or a hydrohalide thereof, (ii) a strong base (e.g., NaOH) in proportions of about 2.0 to about 4.0 moles of (ii) per mole of (i), and (iii) at least one solvent for the base (e.g., H.sub.2 O). To this mixture is added a hydrocarbyl monohalide (e.g., EtBr) in proportions of about 1.0 to about 3.0 moles per mole of phosphoroamidite used in forming the initial mixture, and the resultant reaction produces tetrakis(dihydrocarbylamino)phosphonium halide. The process enables more efficient production of tetrakis(dihydrocarbylamino)phosphonium halides, and is capable of being effectively used in large scale production facilities while satisfying the economic constraints of commercial operations.
摘要翻译： 混合物由（i）三（二烃基氨基）亚氨基亚胺和/或其氢卤化物，（ii）比例为约2.0-约4.0摩尔（ⅱ）每摩尔（ⅰ）的强碱（例如，NaOH） ），和（iii）至少一种用于碱（例如H 2 O）的溶剂。 向该混合物中加入每摩尔用于形成初始混合物的亚磷酰胺约1.0至约3.0摩尔的烃基单卤化物（例如EtBr），所得反应产生四（二烃基氨基）鏻卤化物。 该方法能够更有效地生产四（二烃基氨基）鏻卤化物，并且能够有效地用于大规模生产设备，同时满足商业操作的经济限制。
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公开(公告)号：US5965781A
公开(公告)日：1999-10-12
申请号：US975924
申请日：1997-11-21
申请人： Bruce C. Berris , Chi-Hung Cheng
发明人： Bruce C. Berris , Chi-Hung Cheng
CPC分类号： C07F9/06 , C07C17/208 , C07F9/025
摘要： Impure tetra(dihydrocarbylamino)phosphonium halide is contacted with a liquid cyclic ether to dissolve the phosphonium halide and leave at least a portion of the impurities comprising at least quaternary ammonium halide or an amidophosphoxide remaining in the solid state. The solids and the liquid phase are separated from each other, an anhydrous non-solvent for the tetra(dihydrocarbylamino)phosphonium halide is mixed with the separated liquid phase to precipitate the tetra(dihydrocarbylamino)phosphonium halide, which is then separated from the liquid phase. The so-treated tetra(dihydrocarbylamino)phosphonium halide is more efficient as a catalyst for halogen exchange reactions than the original untreated tetra(dihydrocarbylamino)phosphonium halide.
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4.发明授权
公开(公告)号：US4946975A
公开(公告)日：1990-08-07
申请号：US464312
申请日：1990-01-12
申请人： Feng-Jung Wu , Bruce C. Berris , Donald R. Bell
发明人： Feng-Jung Wu , Bruce C. Berris , Donald R. Bell
IPC分类号： C07F13/00
CPC分类号： C07F13/00
摘要： Cyclopentadienyl manganese tricarbonyl compounds are made by reacting a mixture of 0.25-0.55 moles of manganese acetate and 0.45-0.55 moles of a bis-cyclopentadienyl manganese compound with about 0.5-2.1 moles of an alkyl aluminum compound (e.g. triethyl aluminum) in the presence of about 0.75-1.25 moles of an ether per mole of said alkyl aluminum compound and reacting the mixture with carbon monoxide at about 65.degree.-175.degree. C. and 300-1500 psig.
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公开(公告)号：US20080306302A1
公开(公告)日：2008-12-11
申请号：US12097246
申请日：2006-12-08
申请人： Bruce C. Berris
发明人： Bruce C. Berris
IPC分类号： C07C241/02 , C07F5/02
CPC分类号： C07C241/02 , C07F5/027 , C07C243/22
摘要： A process for the preparation of organic cation tetrakis(Faryl) borate salts. The process includes preparation of intermediate, mono-hydrazine substituted (Faryl) compound, from (Faryl) compound using hydrazine at temperatures below 78° C. A stoichiometric excess of hydrazine to the (Faryl) compound to the (Faryl) compound is used. The process further includes the preparation of the organic cation tetrakis(Faryl) borate in ethereal medium.
摘要翻译： 一种制备有机阳离子四（氟芳基）硼酸盐的方法。 该方法包括使用肼在低于78℃的温度下由（芳基）化合物制备中间体，单肼取代的（芳基）化合物。使用（Faryl）化合物与（芳基）化合物的化学计量过量的肼。 该方法还包括在醚介质中制备有机阳离子四（氟芳基）硼酸盐。
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公开(公告)号：US6046358A
公开(公告)日：2000-04-04
申请号：US351888
申请日：1999-07-13
申请人： Bruce C. Berris , Chi-Hung Cheng
发明人： Bruce C. Berris , Chi-Hung Cheng
CPC分类号： C07F9/06 , C07C17/208 , C07F9/025
摘要： Impure tetra(dihydrocarbylamino)phosphonium halide is contacted with a liquid cyclic ether to dissolve the phosphonium halide and leave at least a portion of the impurities comprising at least quaternary ammonium halide or an amidophosphoxide remaining in the solid state. The solids and the liquid phase are separated from each other, an anhydrous non-solvent for the tetra(dihydrocarbylamino)phosphonium halide is mixed with the separated liquid phase to precipitate the tetra(dihydrocarbylamino)phosphonium halide, which is then separated from the liquid phase. The so-treated tetra(dihydrocarbylamino)phosphonium halide is more efficient as a catalyst for halogen exchange reactions than the original untreated tetra(dihydrocarbylamino)phosphonium halide.
摘要翻译： 不纯的四（二烃基氨基）鏻卤化物与液体环状醚接触以溶解卤化鏻，并使至少一部分杂质至少包含季铵卤化物或酰胺二氧化物保持在固态。 将固体和液相彼此分离，用于四（二烃基氨基）鏻卤化物的无水非溶剂与分离的液相混合以沉淀四（二烃基氨基）鏻卤化物，然后将其从液相中分离出来 。 如此处理的四（二烃基氨基）鏻卤化物作为卤素交换反应的催化剂比原始未处理的四（二烃基氨基）鏻卤化物更有效。
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公开(公告)号：US5292969A
公开(公告)日：1994-03-08
申请号：US41097
申请日：1993-04-01
申请人： Bruce C. Berris
发明人： Bruce C. Berris
CPC分类号： C07C37/16
摘要： A 1,3,5-trimethyl-2,4,6-tris(3,5-dialkyl-4-hydroxybenzyl)benzene is prepared in high yield by reacting a 2,6-dialkyl-4-methoxymethylphenol with mesitylene in a hydrocarbon solvent and in the presence of at least about 10 mol %, based on the amount of mesitylene, of a hydrocarbon-soluble acid (e.g., an alkylbenzenesulfonic acid having 12-18 carbons in the alkyl group, a carboxylic acid, or a dialkylsulfosuccinate) as a catalyst or co-catalyst while distilling methanol by-product out of the reaction mixture as it is formed. The process may be conducted so as to provide a substantially pure product or a product, such as 1,3,5-trimethyl-2,4,6-tris(3,5-di-t-butyl-4-hydroxybenzyl)benzene, having fairly high purity (e.g., about 98-98%) and a melting point much lower than would be expected of a product having such high purity.
摘要翻译： 通过使2,6-二烷基-4-甲氧基甲基苯酚与均三甲苯在烃中反应，以高产率制备1,3,5-三甲基-2,4,6-三（3,5-二烷基-4-羟基苄基）苯 基于均三甲苯的量，至少约10mol％的烃溶性酸（例如烷基中具有12-18个碳的烷基苯磺酸，羧酸或二烷基磺基琥珀酸盐）存在下， 作为催化剂或助催化剂，同时在其形成时从反应混合物中蒸馏甲醇副产物。 该方法可以进行以提供基本上纯的产物或产物，例如1,3,5-三甲基-2,4,6-三（3,5-二叔丁基-4-羟基苄基）苯 ，具有相当高的纯度（例如，约98-98％），熔点远低于具有如此高纯度的产品的熔点。
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公开(公告)号：US20110301395A1
公开(公告)日：2011-12-08
申请号：US13131773
申请日：2009-10-28
IPC分类号： C07C5/42
CPC分类号： C07C5/367 , C07C2523/42 , C07C2523/44 , C07C2603/42 , C07C15/38
摘要： Processes are provided for producing triphenylene by combining at least dodecahydrotriphenylene, a dehydrogenation catalyst such as palladium on carbon, and an aliphatic solvent having a boiling point greater than 180° C. to form a reaction mixture, heating the reaction mixture to at least about 180° C. but lower than the boiling point of the aliphatic solvent, maintaining the temperature of the reaction mixture at 180° C. but lower than the boiling point of the aliphatic solvent, and passing a purge fluid comprising an inert fluid through the reaction mixture, for a period of time adequate for production of triphenylene.
摘要翻译： 提供了通过将至少十二氢三亚苯，脱氢催化剂如钯碳和沸点大于180℃的脂族溶剂组合形成反应混合物来生产聚苯乙烯的方法，将反应混合物加热至至少约180℃ ℃，但低于脂族溶剂的沸点，将反应混合物的温度保持在180℃但低于脂族溶剂的沸点，并将包含惰性流体的清洗流体通过反应混合物 ，一段时间足以生产三亚苯。
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公开(公告)号：US5089648A
公开(公告)日：1992-02-18
申请号：US577280
申请日：1990-09-04
申请人： Bruce C. Berris
发明人： Bruce C. Berris
CPC分类号： C07F7/0896 , C07F7/0801 , C07F7/21
摘要： Improved methods for producing polysilane compounds using tetrakis(triethylphosphine)nickel (O) catalysts.
摘要翻译： 使用四（三乙基膦）镍（O）催化剂生产聚硅烷化合物的改进方法。
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公开(公告)号：US08575412B2
公开(公告)日：2013-11-05
申请号：US13131773
申请日：2009-10-28
IPC分类号： C07C5/367
CPC分类号： C07C5/367 , C07C2523/42 , C07C2523/44 , C07C2603/42 , C07C15/38
摘要： Processes are provided for producing triphenylene by combining at least dodecahydrotriphenylene, a dehydrogenation catalyst such as palladium on carbon, and an aliphatic solvent having a boiling point greater than 180° C. to form a reaction mixture, heating the reaction mixture to at least about 180° C. but lower than the boiling point of the aliphatic solvent, maintaining the temperature of the reaction mixture at 180° C. but lower than the boiling point of the aliphatic solvent, and passing a purge fluid comprising an inert fluid through the reaction mixture, for a period of time adequate for production of triphenylene.
摘要翻译： 提供了通过将至少十二氢三亚苯，脱氢催化剂如钯碳和沸点大于180℃的脂族溶剂组合形成反应混合物来生产聚苯乙烯的方法，将反应混合物加热至至少约180℃ ℃，但低于脂族溶剂的沸点，将反应混合物的温度保持在180℃但低于脂族溶剂的沸点，并将包含惰性流体的清洗流体通过反应混合物 ，一段时间足以生产三亚苯。
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