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1. 发明授权

US4987229A Purification of salts of riboflavin 5'-phosphate, in particular of monosodium riboflavin 5'-phosphate 失效
标题翻译：核黄素5'-磷酸盐，特别是核黄素5'-磷酸一钠的盐的纯化
公开(公告)号：US4987229A
公开(公告)日：1991-01-22
申请号：US323795
申请日：1989-03-15
申请人： Walter Dobler , Manfred Eggersdorfer , Joachim Paust
发明人： Walter Dobler , Manfred Eggersdorfer , Joachim Paust
IPC分类号： C07D475/14 , C07F9/6561
CPC分类号： C07F9/65618
摘要： Salts of riboflavin 5'-phosphate which are obtained by phosphorylation of riboflavin and reaction of the resulting riboflavin 5'-phosphate (5'-FMN), contaminated with unconverted riboflavin and isomeric riboflavin monophosphates and diphosphates, with an alkali metal hydroxide or a nitrogen base are purified by a process in which(a) a roughly 1-15% strength by weight homogeneous, clear, aqueous 5'-FMN salt solution having a pH of from 4 to 7 is prepared from the crude 5'-FMN obtained in the phosphorylation, water and the alkali metal hydroxide or the nitrogen base, preferably sodium hydroxide solution, if necessary with heating at from 30.degree. to 100.degree. C.,(b) the resulting solution is treated with a suitable polymeric adsorber resin and(c) the 5'-FMN salt substantially freed from unconverted riboflavin is isolated from the resulting solution and, if desired, the solution is fed to a subsequent fine purification.Treatment with the suitable polymeric adsorber resin is advantageously carried out in a column filled with adsorber resin. The subsequent fine purification can be effected by evaporative crystallization or by chromatographing a 5'-FMN solution, containing from 1 to 15% by weight of dry substance, in water or in a mixture of water and a lower aliphatic alcohol, having a pH of from 4 to 7, in a minimum amount of from 5 to 50% of the bed volume of the column over RP silica gel derivatized with alkyl groups, using water, or a mixture of water and a lower aliphatic alcohol, as the eluant. Preparative chromatography of 5'-FMN salts over derivatized RP silica gel using water, or a mixture of water and a lower aliphatic alcohol, as the solvent and eluant is also claimed independently of pretreatment with the suitable adsorber resin.
摘要翻译：通过核黄素磷酸化获得的核黄素5'-磷酸盐的盐和由未转化的核黄素和异构核黄素单磷酸酯和二磷酸酯污染的所得核黄素5'-磷酸（5'-FMN）与碱金属氢氧化物或氮碱通过以下方法纯化，其中（a）从所得粗制5'-FMN制备了具有约1-15％重量的均匀，透明的pH5-4的5-FMN盐水溶液，磷酸化，水和碱金属氢氧化物或氮碱，优选氢氧化钠溶液，如果需要，在30℃至100℃下加热，（b）所得溶液用合适的聚合物吸附树脂处理，（c ）从所得溶液中分离出基本上未转化的核黄素的5'-FMN盐，并且如果需要，将溶液加入到随后的精细纯化中。用合适的聚合物吸附树脂处理有利地在填充有吸附树脂的柱中进行。随后的精细纯化可以通过蒸发结晶或通过色谱法将含有1至15重量％干物质的5-FMN溶液在水或水和低级脂族醇的混合物中进行，其pH为作为洗脱剂，使用水或水和低级脂族醇的混合物，用烷基衍生的RP硅胶的柱体积的最小量为5至50％。独立于合适的吸附剂树脂的预处理，也要求使用水，或水和低级脂族醇的混合物作为溶剂和洗脱剂的衍生化RP硅胶的5-FMN盐的制备色谱法。

2. 发明授权

US4999437A Preparation of ascorbic acid 2-phosphate and of 5, 6-isopropylideneascorbic acid and potassium magnesium l-ascorbate 2-phosphate as an advantageous salt of l-ascorbic acid 2- phosphate 失效
标题翻译：作为1-抗坏血酸2-磷酸盐的有利盐，制备抗坏血酸2-磷酸酯和5,6-异丙基亚甲基抗坏血酸和1-抗坏血酸钾钾2-磷酸酯
公开(公告)号：US4999437A
公开(公告)日：1991-03-12
申请号：US486755
申请日：1990-03-01
申请人： Walter Dobler , Joachim Paust , Roland Betz
发明人： Walter Dobler , Joachim Paust , Roland Betz
IPC分类号： C07F9/655
CPC分类号： C07F9/65515
摘要： Ascorbic acid 2-phosphate is prepared by reacting ascorbic acid or an ascorbic acid derivative with POCl.sub.3 in the presence of a tertiary amine in a suitable aqueous solvent at from -10.degree. to 25.degree. C. while maintaining a pH of about 8-13.5 with KOH during the entire phosphorylation reaction and then isolating the ascorbic acid 2-phosphate, by a process in which an aqueous solution of a magnesium compound is added to the reaction mixture obtained in the phosphorylation, without prior treatment with an ion exchanger, until the formation of crystalline KMg PO.sub.4 is complete, the KMgPO.sub.4 which is crystallized out is separated off, the resulting filtrate is evaporated down at a pH of from 6 to 11 and/or from 0.1 to 5 times the amount, based on the evaporated filtrate, of a lower primary alkanol or acetone is added and the stirred mixture is cooled until KCl has completely crystallized out, and the ascorbic acid phosphate is isolated in a conventional manner from the reaction solution obtained by separating off KCl and substantially freed from inorganic salts. It is particularly advantageous if the ascorbic acid 2-phosphate is isolated in the form of the novel potassium magnesium ascorbate 2-phosphate, which is also claimed.The process is particularly advantageous if the ascorbic acid derivative used is 5,6-isopropylideneascorbic acid which has been obtained by reacting ascorbic acid with acetone in the presence of oleum. The process is particularly important for the preparation of L-ascorbic acid 2-phosphate.
摘要翻译：抗坏血酸2-磷酸酯通过使抗坏血酸或抗坏血酸衍生物与POCl 3在叔胺存在下，在-10℃至25℃的合适的水性溶剂中反应制备，同时保持约8-13.5的pH，同时用 KOH，然后通过将镁化合物的水溶液加入到磷酸化中获得的反应混合物中而不用离子交换剂进行预处理的方法分离出抗坏血酸2-磷酸酯，直到形成结晶KMg PO4完成后，将结晶出来的KMgPO4分离出来，所得滤液按照蒸发滤液的6至11和/或0.1至5倍的pH蒸发掉，加入低级主链烷醇或丙酮，将搅拌的混合物冷却直至KCl完全结晶出来，并以常规方式从得到的反应溶液中分离抗坏血酸磷酸酯通过分离KCl并基本上从无机盐中除去。特别有利的是，抗坏血酸2-磷酸酯以新的抗坏血酸钾2-磷酸2-钾的形式被分离，这也是要求保护的。如果所使用的抗坏血酸衍生物是在发烟硫酸存在下使抗坏血酸与丙酮反应获得的5,6-异亚丙基抗坏血酸，该方法是特别有利的。该方法对于制备L-抗坏血酸2-磷酸酯尤为重要。

3. 发明授权

US5344995A Preparation of cyclic acetals of 3-formyl-2-butenyltriphenylphosphonium chloride 失效
标题翻译：制备3-甲酰基-2-丁烯基三苯基氯化鏻的环状缩醛
公开(公告)号：US5344995A
公开(公告)日：1994-09-06
申请号：US85903
申请日：1993-07-06
申请人： Wolfgang Krause , Joachim Paust , Walter Dobler , Hagen Jaedicke
发明人： Wolfgang Krause , Joachim Paust , Walter Dobler , Hagen Jaedicke
IPC分类号： C07F9/54 , C07D319/06 , C07F9/655 , C07C43/305 , C07C43/313
CPC分类号： C07F9/6552 , C07D319/06
摘要： An improved process for preparing cyclic acetals of 3-formyl-2-butenyltriphenylphosphonium chloride by acetalization of 3-formyl-2-butenyl acetate with an aliphatic 1,3-diol, conversion of the resulting 4-acetoxy acetal into the corresponding 4-hydroxy acetal, Vilsmeier chlorination to give the corresponding 4-chloro acetal and subsequent reaction with triphenylphosphine entails carrying out the first 3 steps in an aliphatic or cycloaliphatic hydrocarbon or mixture of hydrocarbons with 6-8 carbons and the reaction with triphenylphosphine in an alkanol with 1-3 carbons and/or in aliphatic or cycloaliphatic hydrocarbon with 6-8 carbons or a corresponding mixture of hydrocarbons. The process is particularly advantageous when conversion of the 4-acetoxy acetal into the 4-hydroxy acetal is carried out with an aqueous alkali metal hydroxide solution in the presence of phase-transfer catalysts, and the first three, or all four, reaction stages are carried out in the same C.sub.6 -C.sub.8 -hydrocarbon.
摘要翻译：通过用脂肪族1,3-二醇缩醛化3-甲酰基-2-丁烯基乙酸酯与3-甲酰基-2-丁烯基三苯基氯化鏻的环状缩醛的改进方法，将得到的4-乙酰氧基缩醛转化为相应的4-羟基缩醛，Vilsmeier氯化，得到相应的4-氯缩醛，随后与三苯基膦反应需要在脂族或脂环族烃或碳原子数为6〜8的混合物中进行前3个步骤，并与三苯基膦在链烷醇中与1- 3个碳原子和/或具有6-8个碳原子的脂族或脂环族烃或相应的烃混合物。当在相转移催化剂存在下，用碱金属氢氧化物水溶液进行4-乙酰氧基缩醛转化为4-羟基缩醛时，该方法是特别有利的，而前三个或所有四个反应阶段是在相同的C6-C8-烃中进行。

4. 发明授权

US5202445A Preparation of potassium magnesium L-ascorbate 2-phosphate 失效
标题翻译：硫酸钾二钠磷酸盐的制备
公开(公告)号：US5202445A
公开(公告)日：1993-04-13
申请号：US747573
申请日：1991-08-20
申请人： Walter Dobler , Hartwig Voss , Friedhelm Balkenhohl , Joachim Paust
发明人： Walter Dobler , Hartwig Voss , Friedhelm Balkenhohl , Joachim Paust
IPC分类号： C07F9/09 , B01D61/44 , C07D307/62 , C07F9/655
CPC分类号： C07D307/62 , C07F9/65515
摘要： Potassium magnesium L-ascorbate 2-phosphate is prepared from an aqueous solution of potassium L-ascorbate 2-phosphate which is highly contaminated with KCl, as is produced in the phosphorylation of 5,6-isopropylidene-L-ascorbic acid, by adding to the solution about 1 equivalent of magnesium ions per equivalent of L-ascorbate 2-phosphate, and subsequently removing the KCl by electrodialysis. The product of this process is a novel salt of L-ascorbic acid 2-phosphate and has very advantageous handling properties.
摘要翻译：钾抗坏血酸钾2-磷酸盐是由KCl高度污染的L-抗坏血酸钾2-磷酸的水溶液制备的，如在5,6-异亚丙基-L-抗坏血酸的磷酸化中产生的那样，加入到溶液中约1当量的镁离子/当量的L-抗坏血酸2-磷酸，然后通过电渗析除去KCl。该方法的产物是L-抗坏血酸2-磷酸的新型盐，具有非常有利的处理性能。

5. 发明授权

US4778531A Epimerization of sugars, in particular of D-arabinose to D-ribose 失效
标题翻译：糖异构化，特别是D-阿拉伯糖对D-核糖
公开(公告)号：US4778531A
公开(公告)日：1988-10-18
申请号：US68171
申请日：1987-06-30
申请人： Walter Dobler , Hansgeorg Ernst , Joachim Paust
发明人： Walter Dobler , Hansgeorg Ernst , Joachim Paust
IPC分类号： C07B61/00 , C07H3/00 , C07H3/02 , C07H1/00 , C13J1/06
CPC分类号： C07H3/02
摘要： Pentoses and hexoses are epimerized by heating sugar dissolved in a solvent in the presence of a molybdenum(VI) compound, by an improved process in which, for the preparation of a sugar having cis OH groups in the 2- or 3-position, of the formula Ia or Ib ##STR1## where R is one of the radicals ##STR2## a homogeneous solution of the corresponding sugar of the formula IIa or IIb ##STR3## is heated to 75.degree.-100.degree. C. in the presence of from 30 to 200 mol %, based on sugar used, of a metal salt of the formula (III)MeX.sub.2 (III)where Me is Mg, Ca, Sr, Ba or Zn and X is Cl or Br, which may or may not contain water of crystallization, and in the presence of from 2 to 20 mol %, based on the sugar used, of a molybdenum(VI) compound.The process is particularly important for the preparation of D-ribose, which is required as an intermediate for vitamin B.sub.2.
摘要翻译：戊糖和己糖通过加热溶解在钼（VI）化合物存在下的溶剂中的糖进行差向异构化，其中通过改进方法，其中为了制备在2-或3-位具有顺式OH基团的糖，式Ia或Ib的化合物，其中R是式IIa或IIb的相应糖的均匀溶液之一的基团之一，在30℃的存在下加热至75℃-100℃ （III）的MeX2（III）的金属盐，其中Me是Mg，Ca，Sr，Ba或Zn，X是Cl或Br，其可以含有或可以不含水的结晶，并且在基于所用糖的2至20摩尔％的存在下，使用钼（VI）化合物。该方法对于制备作为维生素B2的中间体的D-核糖是特别重要的。

6. 发明授权

US5717128A Preparation of alkylesters of 0,0-dialkyl-4-phosphono-2-methyl-2-butenoic acid and alkyl esters of 4-halo-2-methyl-2-butenoic acid containing a high percentage of E isomers 失效
标题翻译：制备0-0-二烷基-4-膦酰基-2-甲基-2-丁烯酸的烷基酯和含有高百分比的E异构体的4-卤代-2-甲基-2-丁烯酸的烷基酯
公开(公告)号：US5717128A
公开(公告)日：1998-02-10
申请号：US535637
申请日：1995-09-28
申请人： Wolfgang Krause , Hansgeorg Ernst , Joachim Paust , Udo Rheude , Walter Dobler
发明人： Wolfgang Krause , Hansgeorg Ernst , Joachim Paust , Udo Rheude , Walter Dobler
IPC分类号： C07C67/307 , C07F9/40 , C07C69/65
CPC分类号： C07F9/4015 , C07C67/307
摘要： A process for the preparation of alkyl esters of 0,0-dialkyl-4-phosphono-2-methyl-2-butenoic acid containing a high percentage of E isomers, wherein the corresponding alkyl esters of 2-hydroxy-2-methyl-3-butenoic acid are caused to react with PBr.sub.3 or PCl.sub.3 at temperatures ranging from 0.degree. to 80.degree. C. in the absence of pyridine and, if desired, the resulting mixture comprising predominantly alkyl esters of 4-halo-2-methyl-2-butenoic acid is caused to react with trialkyl esters of phosphorous acid at temperatures ranging from 70.degree. to 140.degree. C. The end products are desirable C.sub.5 building blocks for polyene syntheses or preceding stages.
摘要翻译：一种制备含有高百分比的E异构体的0-二烷基-4-膦酰基-2-甲基-2-丁烯酸的烷基酯的方法，其中相应的2-羟基-2-甲基-3 在不存在吡啶的情况下，在0℃至80℃的温度范围内引发 - 丁烯酸与PBr 3或PCl 3反应，如果需要，所得混合物主要包含4-卤代-2-甲基-2- 使丁烯酸在70℃至140℃的温度范围内与亚磷酸三烷基酯反应。最终产物是用于多烯合成或先前阶段的所需C5构建块。

7. 发明授权

US5489694A Preparation of R/S-.gamma.-lipoic acid or R/S-.alpha.-lipoic acid 失效
公开(公告)号：US5489694A
公开(公告)日：1996-02-06
申请号：US279418
申请日：1994-07-25
申请人： Joachim Paust , Peter Eckes , Wolfgang Siegel , Friedhelm Balkenhohl , Walter Dobler , Michael Hullmann
发明人： Joachim Paust , Peter Eckes , Wolfgang Siegel , Friedhelm Balkenhohl , Walter Dobler , Michael Hullmann
IPC分类号： C07C69/708 , C07C319/08 , C07C323/52 , C07D313/04 , C07D339/04 , C07C53/126
CPC分类号： C07C69/708 , C07C319/08 , C07D313/04 , C07D339/04
摘要： A process for preparing R/S-.gamma.-lipoic acid of the formula I or R/S-.alpha.-lipoic acid of the formula II ##STR1## is disclosed.

8. 发明授权

US5455362A Preparation of astaxanthin novel intermediates therefor and the preparation thereof 失效
标题翻译：虾青素的制备方法及其制备方法
公开(公告)号：US5455362A
公开(公告)日：1995-10-03
申请号：US265741
申请日：1994-06-27
申请人： Hansgeorg Ernst , Walter Dobler , Joachim Paust , Udo Rheude
发明人： Hansgeorg Ernst , Walter Dobler , Joachim Paust , Udo Rheude
IPC分类号： C07C41/18 , C07C45/45 , C07C49/303 , C07C403/24 , C07D317/46 , C07D317/50 , C07D317/54 , C07D407/06 , C07D407/12 , C07F9/54 , C09B23/10
CPC分类号： C07C403/24 , C07C403/04 , C07C403/08 , C07C403/10 , C07D317/46 , C07F9/5435 , C07F9/5442 , C07C2101/16 , Y02P20/55
摘要： Compounds of the formula I ##STR1## where R.sup.1 is H or C.sub.1 -C.sub.4 -alkyl,R.sup.2 is C.sub.1 -C.sub.4 -alkyl and R.sup.3 is an ether, silyl ether or acetal protective group which can be converted into a hydroxyl group by hydrolysis, in particular one of the radicals ##STR2## and a process for preparing these compounds by reacting an alkenyne of the formula II ##STR3## in an inert solvent in the presence of lithium amide with a cyclohexenone of the formula III ##STR4## and the use of the compounds of the formula I for preparing astaxanthin, are described.
摘要翻译：其中R 1是H或C 1 -C 4 - 烷基，R 2是C 1 -C 4 - 烷基和R 3是醚的式I化合物（I），甲硅烷基醚或缩醛保护基，其可以通过以下方式转化成羟基：水解，特别是一个基团“IMAGE”，以及通过在惰性溶剂中在酰胺与式III的环己烯酮的存在下使式II的烯烃（II）反应来制备这些化合物的方法， IMAGE>（III）和使用式I化合物制备虾青素。

9. 发明授权

US5773635A Preparation of polyenecarbonyl compounds having a high content of the all-E isomer, and of their acetals or ketals 失效
标题翻译：具有全E异构体含量高的多烯羰基化合物及其缩醛或缩酮的制备
公开(公告)号：US5773635A
公开(公告)日：1998-06-30
申请号：US498840
申请日：1995-07-06
申请人： Walter Dobler , Wolfgang Krause , Joachim Paust , Otto Worz , Udo Rheude , Wolfram Burst , Gunter Dauwel , Armin Bertram , Bernhard Schulz , Gunter Wegner , Peter Munster , Hansgeorg Ernst , Arno Kochner , Heinz Etzrodt
发明人： Walter Dobler , Wolfgang Krause , Joachim Paust , Otto Worz , Udo Rheude , Wolfram Burst , Gunter Dauwel , Armin Bertram , Bernhard Schulz , Gunter Wegner , Peter Munster , Hansgeorg Ernst , Arno Kochner , Heinz Etzrodt
IPC分类号： C07C51/16 , C07C403/00 , C07C403/20
CPC分类号： C07C403/20 , C07C403/16 , C07B2200/09 , C07C2101/16
摘要： A process for preparing polyenecarbonyl compounds having a high all-E content and their acetals or ketals by aldol condensation or Horner-Emmons reaction comprises carrying out the reaction, for the purposes of the preferred formation of a double bond of E configuration and in order to maintain the E configuration of the double bonds in the stating compounds as completely as possible, in the presence of oxygen or an oxygen-inert gas mixture or nitric oxide or a nitric oxide-inert gas mixture and/or in the presence of specific stable radicals and/or in the presence of quinones or quinone derivatives.
摘要翻译：通过醛醇缩合或霍纳 - 埃蒙斯反应制备具有高全E含量的多元羰基化合物及其缩醛或缩酮的方法包括进行反应，为了优选形成E构型的双键，为了在氧气或氧惰性气体混合物或一氧化氮或一氧化氮惰性气体混合物的存在下和/或在特定的稳定基团的存在下，尽可能地完全地保持化合物中双键的E构型和/或在醌或醌衍生物的存在下。

10. 发明授权

US5654444A Preparation of 5-hydroxy-4-methyl-2(5H)-furanone 失效
标题翻译：制备5-羟基-4-甲基-2（5H） - 呋喃酮
公开(公告)号：US5654444A
公开(公告)日：1997-08-05
申请号：US621035
申请日：1996-03-22
申请人： Michael John , Walter Dobler , Joachim Paust
发明人： Michael John , Walter Dobler , Joachim Paust
IPC分类号： C07D307/60
CPC分类号： C07D307/60
摘要： 5-Hydroxy-4-methyl-2(5H)-furanone is prepared by cyclization of alkyl .beta.-formylcrotonates by heating with dilute aqueous hydrochloric acid or, advantageously, in the presence of dilute aqueous hydrochloric acid and catalytic amounts of methanol as solubilizer, subsequent workup of the reaction mixture by distillation and, where appropriate, isomerization of the 5-methoxy- or 5-ethoxy-4-methyl-2(5H)-furanone, which is formed as byproduct, by heating with dilute hydrochloric acid.
摘要翻译： 5-羟基-4-甲基-2（5H） - 呋喃酮是通过用稀盐酸水溶液加热或有利地在稀盐酸水溶液和催化量的甲醇作为增溶剂的存在下，通过环化β-甲酰基巴豆酸烷基酯来制备的，随后通过蒸馏和通过用稀盐酸加热作为副产物形成的5-甲氧基 - 或5-乙氧基-4-甲基-2（5H） - 呋喃酮的异构化反应混合物进行后处理。

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