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1. 发明授权

US4550182A Preparation of .alpha.-tocopherol 失效
标题翻译： α-生育酚的制备
公开(公告)号：US4550182A
公开(公告)日：1985-10-29
申请号：US588374
申请日：1984-03-12
申请人： Hansgeorg Ernst , Henning-Peter Gehrken , Joachim Paust
发明人： Hansgeorg Ernst , Henning-Peter Gehrken , Joachim Paust
IPC分类号： C07D317/60 , B01J31/16 , C07B61/00 , C07D311/72
CPC分类号： C07D311/72
摘要： A process for the preparation of .alpha.-tocopherol of the formula I ##STR1## by reacting a chroman derivative with a C.sub.14 -Grignard reagent using a di-alkali metal tetrahalocuprate catalyst in a Schlosser-Fouquet reaction, wherein a chroman derivative of the general formula II ##STR2## where Y is a leaving group, especially Br, is used and is reacted, at from -70.degree. to 0.degree. C., first with a solution of about 1 equivalent of a Grignard compound of the general formula IIIX--Mg--R (III)where X is Cl, Br or I and R is straight-chain or branched alkyl of 1 to 14 carbon atoms, preferably methyl, ethyl or ##STR3## and then with a solution of a Grignard reagent of the formula IIIa ##STR4## in an ether solvent and a solution of a di-alkali metal tetrahalocuprate in an ether solvent. The novel process simplifies the preparation of 2RS,4'RS,8'RS-, 2R,4'RS,8'RS- or 2R,4'R,8'R-.alpha.-tocopherol by reacting a chroman structural unit, containing a C.sub.2 side-chain in the 2-position, with the corresponding C.sub.14 -Grignard compound.
摘要翻译：通过在Schlosser-Fouquet反应中使用二碱金属四卤代硼酸催化剂使苯并二氢吡喃衍生物与C14-格氏试剂反应制备式I的α-生育酚的方法，其中将使用其中Y为离去基团，特别是Br的通式II（II），并且在-70℃至0℃下反应，首先用约1当量的Grignard化合物通式III X-Mg-R（III）其中X为Cl，Br或I，R为1至14个碳原子的直链或支链烷基，优选为甲基，乙基或者“ 式IIIa的格利雅试剂（IIIa）在醚溶剂中和二碱金属四卤代硼酸酯在醚溶剂中的溶液。该新方法简化了2RS，4'RS，8'RS-，2R，4'RS，8'RS-或2R，4'R，8'R-α-生育酚的制备，通过使色结构单元反应， 2-位的C2侧链与相应的C14-格利雅化合物。

2. 发明授权

US4645845A Novel optically active chroman derivatives, their preparation and novel intermediates 失效
标题翻译：新型光学活性苯并二氢吡喃衍生物，其制备和新型中间体
公开(公告)号：US4645845A
公开(公告)日：1987-02-24
申请号：US588365
申请日：1984-03-12
申请人： Henning-Peter Gehrken , Hansgeorg Ernst , Joachim Paust
发明人： Henning-Peter Gehrken , Hansgeorg Ernst , Joachim Paust
IPC分类号： C07D311/58 , C07D311/72
CPC分类号： C07D311/72
摘要： Novel optically active chroman derivatives of the general formulae Ia and Ib ##STR1## where R.sup.1, R.sup.2, R.sup.3 and R.sup.4 are each hydrogen or alkyl and X is --OH, --O--CO-alkyl, --O-alkyl, --O-tosyl, --O-mesyl, --O-benzenesulfonyl, Cl, Br or I, are prepared by a process in which(a) the racemate of the formula I' ##STR2## is esterified in the side chain with a carboxylic acid and then acylated with an optically active carboxylic acid halide of the general formula III ##STR3## or with the corresponding carboxylic anhydride, to give a chroman derivative IV ##STR4## or (b) the racemate I' is esterified in the side chain with the carboxylic acid from which III is derived, and, if required, the resulting ester is acylated with a carboxylic acid halide to give IV' ##STR5## the resulting mixture IV or IV', which consists of two diastereomers, is resolved by fractional crystallization, the diastereomers are hydrolyzed to the alcohols Ia and Ib and, if desired, these are converted to the other compounds Ia and Ib in a conventional manner.Useful optically active chroman derivatives Ia and Ib and diastereomeric chromanyl esters IV and IV' are also claimed.
摘要翻译：（Ia）其中R 1，R 2，R 3和R 4各自为氢或烷基且X为-OH，-O-CO-烷基，（C 1 -C 6）烷氧基， -O-烷基，-O-甲苯磺酰基，-O-甲磺酰基，-O-苯磺酰基，Cl，Br或I是通过以下方法制备的，其中（a）式I'（I'）的外消旋物在侧链中用羧酸酯化，然后用通式III（III）的光学活性羧酸卤化物或相应的羧酸酐进行酰化，得到苯并二氢吡喃衍生物IV（IV）或（b）外消旋物I'在侧链中与衍生自其的羧酸酯化，如果需要，将所得酯用羧酸卤化物酰化，得到IV'（IV'）由两个非对映异构体组成的所得混合物IV或IV'通过分级结晶来拆分，非对映异构体被水解成醇Ia和Ib，如果需要，它们是转化的以常规方式与其它化合物Ia和Ib反应。还要求有用的光学活性色氨酸衍生物Ia和Ib以及非对映异构的色满基酯IV和IV'。

3. 发明授权

US06716789B1 Method for producing oxidic catalysts containing copper with oxidation number>0 失效
标题翻译：生产含氧化值> 0的铜的氧化催化剂的方法
公开(公告)号：US06716789B1
公开(公告)日：2004-04-06
申请号：US09581988
申请日：2000-06-21
申请人： Daniel Heineke , Ruprecht Meissner , Michael Hesse , Henning-Peter Gehrken
发明人： Daniel Heineke , Ruprecht Meissner , Michael Hesse , Henning-Peter Gehrken
IPC分类号： B01J2108
CPC分类号： C07C45/002 , B01J23/72 , B01J37/0203 , C07C49/403
摘要： The disclosure is directed to a process for preparing an oxidic catalyst comprising copper in an oxidation state >0, which comprises treating a solid oxidic support material with an aqueous solution comprising at least one copper salt and at least one organic water soluble polymer which binds copper ions coordinatively in a concentration of from 0.1 to 100 g/l and then calcining, to the catalyst obtainable by this process and also to a process for dehydrogenating secondary alcohols to ketones using the catalysts, especially for dehydrogenating cyclohexanol.
摘要翻译：本发明涉及制备氧化态> 0的铜的氧化催化剂的方法，该方法包括用包含至少一种铜盐和至少一种与铜结合的有机水溶性聚合物的水溶液处理固体氧化载体材料离子以0.1至100g / l的浓度配位，然后煅烧至可通过该方法获得的催化剂，并且还涉及一种使用催化剂，特别是用于使环己醇脱氢来将仲醇脱氢成酮的方法。

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