公开(公告)号：US4681936A

公开(公告)日：1987-07-21

申请号：US826317

申请日：1986-02-05

申请人： Klaus-Peter Pfaff ,  Joachim Paust ,  Horst Hartmann

发明人： Klaus-Peter Pfaff ,  Joachim Paust ,  Horst Hartmann

IPC分类号： C07H1/00 ,  B01J31/00 ,  C07B61/00 ,  C07H9/04

CPC分类号： C07H9/04

摘要： Sugar ketals are prepared by reacting a sugar with a ketone in the presence of an acid catalyst by a process in whichA. a molecular boron trifluoride compound or trifluoromethanesulfonic acid is used in an amount of only from 0.01 to 10% by weight, based on the sugar used,B. up to a 30-fold molar excess of the ketone is used andC. the water formed during the reaction is removed continuously from the reaction mixture.In a particularly advantageous embodiment of the process, the boron trifluoride is used in the form of boron trifluoride etherate and, when the reaction is complete, this compound or the trifluoromethanesulfonic acid is rendered ineffective under non-aqueous conditions, after which the ketone is evaporated off and the reaction mixture is then subjected to fractional distillation. The process is particularly important for the reaction of L-sorbose with acetone to obtain 2,3:4,6-di-O-isopropylidene-L-sorbofuranose, which is required for the synthesis of ascorbic acid.

摘要翻译： 糖缩成物是通过在酸催化剂存在下使糖与酮反应的方法制备的，其中A为分子三氟化硼化合物或三氟甲磺酸的用量，其量仅为0.01至10重量％，基于 使用的糖，B.使用高达30倍摩尔过量的酮，并且C.从反应混合物中连续除去反应期间形成的水。 在该方法的特别有利的实施方案中，三氟化硼以三氟化硼醚合物的形式使用，当反应完成时，该化合物或三氟甲磺酸在非水性条件下变得无效，之后酮蒸发 然后将反应混合物进行分馏。 该方法对于L-山梨糖与丙酮的反应特别重要，得到合成抗坏血酸所需的2,3：4,6-二-O-异亚丙基-L-山梨糖。

公开(公告)号：US5777173A

公开(公告)日：1998-07-07

申请号：US751947

申请日：1996-11-19

申请人： Joachim Paust ,  Wolfgang Kriegl ,  Horst Hartmann

发明人： Joachim Paust ,  Wolfgang Kriegl ,  Horst Hartmann

IPC分类号： C07B57/00 ,  C07C45/82 ,  C07C49/497

CPC分类号： C07C45/82

摘要： A process for the preparation of pure trans- and cis-4-hydroxy-2, 2,6-trimethylcyclohexan-1-one from a mixture of these isomers comprises fractionally rectifying the isomeric mixture in a suitable column having from about 30 to 80 theoretical separation stages at temperatures of preferably from 50.degree. to 130.degree. C. and a pressure in the range from 0.1 to 5 mbar. The products are essential intermediates for the preparation of 3-hydroxycarotenoids such as cryptoxanthin and zeaxanthin.

摘要翻译： 从这些异构体的混合物制备纯的反式和顺式-4-羟基-2,2,6-三甲基环己烷-1-酮的方法包括在合适的柱中对具有约30至80个理论值的合成柱进行分级精馏 优选在50至130℃的温度和0.1至5毫巴范围内的压力下进行分离。 该产品是制备3-羟基类胡萝卜素如隐黄质和玉米黄质的重要中间体。

公开(公告)号：US5654488A

公开(公告)日：1997-08-05

申请号：US616459

申请日：1996-03-15

申请人： Wolfgang Krause ,  Klaus Henrich ,  Joachim Paust ,  Hansgeorg Ernst

发明人： Wolfgang Krause ,  Klaus Henrich ,  Joachim Paust ,  Hansgeorg Ernst

IPC分类号： C07C45/00 ,  C07C47/21 ,  C07C403/24 ,  C07F9/52

CPC分类号： C07C403/24

摘要： Improved process for the preparation of astaxanthin by Wittig reaction of 2 mol of 3-methyl-5-(2,6,6-trimethyl-3-oxo-4-hydroxy-1-cyclohexenyl)-2,4-pentadienyltriarylphosphonium salts with one mol of 2,7-dimethyl-2,4,6-octatrienedial avoiding the use of halohydrocarbons as solvents.

摘要翻译： 通过2摩尔3-甲基-5-（2,6,6-三甲基-3-氧代-4-羟基-1-环己烯基）-2,4-戊二烯基三芳基鏻盐与一摩尔的Wittig反应制备虾青素的改进方法 摩尔的2,7-二甲基-2,4,6-八辛酸，避免使用卤代烃作为溶剂。

公开(公告)号：US5530143A

公开(公告)日：1996-06-25

申请号：US381424

申请日：1995-01-31

申请人： Friedhelm Balkenhohl ,  Joachim Paust

发明人： Friedhelm Balkenhohl ,  Joachim Paust

IPC分类号： C07C67/31 ,  C07C69/675 ,  C07C69/716 ,  C07D339/04 ,  C12N1/18 ,  C12P7/62 ,  C07C69/66

CPC分类号： C07C67/31

摘要： (6S)-6,8-Dihydroxyoctanoic esters I ##STR1## (R.sup.1 =alkyl, cycloalkyl, aralkyl or aryl), are prepared by reducing a (3S)-3-hydroxyoctanedioic diester II ##STR2## (R.sup.2 =an R.sup.1 radical group) with a complex hydride and are mainly used as intermediates for synthesizing compounds of the type of liponic acid.

摘要翻译： 通过还原（3S）-3-羟基辛二酸二酯II（R 2 = R 1）制备（6S）-6,8-二羟基辛酸酯I（R1 =烷基，环烷基，芳烷基或芳基） 自由基基团），并且主要用作合成脂肪酸类化合物的中间体。

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。

公开(公告)号：US5294731A

公开(公告)日：1994-03-15

申请号：US36023

申请日：1993-03-23

申请人： Joachim Paust ,  Wolfgang Siegel

发明人： Joachim Paust ,  Wolfgang Siegel

IPC分类号： C07C67/343 ,  C07C69/76 ,  C07C69/66

CPC分类号： C07C67/343

摘要： A process for the preparation of .beta.-hydroxycarboxylates of the general formula I ##STR1## in which R.sup.1 and R.sup.2 individually denoteC.sub.1 -C.sub.20 alkyl optionally substituted by C.sub.1 -C.sub.8 alkoxy and/or halogen, C.sub.3 -C.sub.20 alkoxycarbonylalkyl, C.sub.2 -C.sub.20 alkenyl, C.sub.5 -C.sub.30 acetalalkenyl, aryl optionally mono- to penta-substituted by C.sub.1 -C.sub.8 alkyl, C.sub.1 -C.sub.8 alkoxy, and/or halogen, C.sub.7 -C.sub.20 aralkyl, C.sub.7 -C.sub.20 aralkenyl, hetaryl, C.sub.3 -C.sub.20 cycloalkyl, or C.sub.4 -C.sub.20 cycloalkylalkyl,or together denote a C.sub.2 -C.sub.8 alkylene chainand one or other of R.sup.1 and R.sup.2 denotes hydrogen, andR.sup.3 denotes hydrogen, C.sub.1 -C.sub.20 alkyl, C.sub.2 -C.sub.20 alkenyl, aryl optionally mono- to penta-substituted by C.sub.1 -C.sub.8 alkyl, C.sub.1 -C.sub.8 alkoxy, and/or halogen, C.sub.7 -C.sub.20 aralkyl, C.sub.3 -C.sub.20 cycloalkyl, or C.sub.4 -C.sub.20 cycloalkylalkyl, andR.sup.4 denotes C.sub.1 -C.sub.20 alkyl, C.sub.4 -C.sub.20 alkenyl, C.sub.7 -C.sub.20 aralkyl, C.sub.3 -C.sub.20 cycloalkyl, or C.sub.4 -C.sub.20 cycloalkylalkyl,by the reaction of carbonyl compounds of the general formula II ##STR2## in which R.sup.1 and R.sup.2 have the meanings stated above, with .alpha.-bromocarboxylates of the general formula III ##STR3## in which R.sup.3 and R.sup.4 have the meanings stated above, wherein the reaction with zinc is carried out in methylene chloride at a temperature ranging from 0.degree. to 50.degree. C.

摘要翻译： 制备通式I（I）的β-羟基羧酸盐的方法，其中R 1和R 2各自表示任选被C 1 -C 8烷氧基和/或卤素取代的C 1 -C 20烷基，C 3 -C 20烷氧基羰基烷基， C20烯基，C5-C30乙缩醛基，C1-C8烷基，C1-C8烷氧基和/或卤素任选被一至五取代的芳基，C 7 -C 20芳烷基，C 7 -C 20芳烯基，杂芳基，C 3 -C 20环烷基或 C 4 -C 20环烷基烷基，或一起表示C 2 -C 8亚烷基链，R 1和R 2中的一个或其中R 1表示氢，R 3表示氢，C 1 -C 20烷基，C 2 -C 20链烯基，任选地被C1任意单 - 五取代的芳基 C 8烷基，C 1 -C 8烷氧基和/或卤素，C 7 -C 20芳烷基，C 3 -C 20环烷基或C 4 -C 20环烷基烷基，R 4表示C 1 -C 20烷基，C 4 -C 20烯基，C 7 -C 20芳烷基， C20环烷基或C4-C20环烷基烷基，通过其中R1和R2具有上述含义的通式II（II）的羰基化合物与α-溴代羰基 通式III的化合物（III）其中R3和R4具有上述含义，其中与二氯甲烷的反应在0℃至50℃的温度下进行。

公开(公告)号：US5210314A

公开(公告)日：1993-05-11

申请号：US695336

申请日：1991-04-29

申请人： Hansgeorg Ernst ,  Joachim Paust ,  Werner Hoffmann

发明人： Hansgeorg Ernst ,  Joachim Paust ,  Werner Hoffmann

IPC分类号： C07C45/75 ,  C07C49/653 ,  C07C49/743 ,  C07C69/63 ,  C07C403/12 ,  C07C403/24 ,  C07F9/54

CPC分类号： C07C403/24 ,  C07C403/12 ,  C07F9/54 ,  C07F9/5435 ,  C07C2101/16

摘要： A process for preparing canthaxanthin (Ia) and astaxanthin (Ib) of the formula I ##STR1##where R is H (a) or OH (b), comprises reacting a tertiary alcohol of the formula II ##STR2##where R is H (a) or OH (b), with trifluoroacetic acid, reacting the resulting novel trifluoroacetate of the formula III ##STR3##with triphenylphosphine, and reacting the resulting novel triphenylphosphonium trifluoroacetate of the formula IV ##STR4## with 2,7-dimethyl-2,4,6-octatriene-1,8-dial under the conditions of a Wittig synthesis. The present invention also relates to the novel trifluoroacetates of the formula III and the corresponding triphenylphosphonium trifluoroacetates of the formula IV.

摘要翻译： 制备式I的角黄素（Ia）和虾青素（Ib）的方法，其中R是H（a）或OH（b））包括使式II的叔醇（II）与R （III）的三氟乙酸盐与三苯基膦反应，并使得到的式IV的三氟化三苯基鏻（Ⅳ）与式（Ⅳ）化合物反应，得到新的三氟乙酸盐， 在Wittig合成条件下用2,7-二甲基-2,4,6-辛二烯-1,8-表盘。 本发明还涉及式III的新型三氟乙酸盐和式Ⅳ相应的三苯基三氟乙酸盐。

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。

公开(公告)号：US4918191A

公开(公告)日：1990-04-17

申请号：US393976

申请日：1989-08-15

申请人： Joachim Paust ,  Hansgeorg Ernst

发明人： Joachim Paust ,  Hansgeorg Ernst

IPC分类号： C07D239/42

CPC分类号： C07D239/42

摘要： In an improved process for the preparation of 2-n-propyl-4-amino-5-methoxymethyl-pyrimidine of the formula I ##STR1## by reacting butyramidine II ##STR2## with .alpha.-methoxymethyl-.beta.-methoxyacrylonitrile III ##STR3## the butyramidine II is reacted with a 0.4-5 molar excess of .alpha.-methoxymethyl-.beta.-methoxyacrylonitrile III at from -10.degree. to +20.degree. C.

摘要翻译： 通过使丁酰脒II II与α​​-甲氧基甲基-β-甲氧基丙烯腈III反应制备式I的2-正丙基-4-氨基-5-甲氧基甲基 - 嘧啶的改进方法III IMA图 > III，在-10℃至+ 20℃下，使丁酰脒II与0.4-5摩尔过量的α-甲氧基甲基-β-甲氧基丙烯腈III反应。

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。