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    Purification of esters of tetrahydro-pyran-4-carboxylic acid
    2.
    发明授权
    Purification of esters of tetrahydro-pyran-4-carboxylic acid 失效
    四氢 - 吡喃-4-羧酸酯的纯化

    公开(公告)号：US5414097A

    公开(公告)日：1995-05-09

    申请号：US185179

    申请日：1994-01-24

    申请人： Rolf Fischer ,  Norbert Goetz ,  Thomas Kuekenhoehner ,  Harald Rust ,  Werner Schnurr

    发明人： Rolf Fischer ,  Norbert Goetz ,  Thomas Kuekenhoehner ,  Harald Rust ,  Werner Schnurr

    IPC分类号： C07D309/08

    CPC分类号： C07D309/08

    摘要： A process for purifying esters of tetrahydropyran-4-carboxylic acid of the formula I ##STR1## where R.sup.1 to R.sup.3 are each C.sub.1 -C.sub.4 -alkyl, and R.sup.2 and R.sup.3 are each additionally hydrogen, from mixtures produced in the reaction of butyrolactones of the formula II ##STR2## where R.sup.2 and R.sup.3 have the abovementioned meanings, and R.sup.4 is hydrogen, alkyl of 1-6 carbons or acyl of the formula --CO--R.sup.2, with alcohols of the formula R.sup.1 OH in the presence of oxide catalysts, by distillation, which entailsa) removing overhead, in a first column with 5-25 theoretical plates with a distillate pressure of 700-1100 mbar and a distillate temperature of 50.degree.-80.degree. C., an alcohol and up to 10% of the water,b) transferring the bottom product from the first column into a second column with 18-40 theoretical plates, into which a water entrainer is metered between plates 15 and 30, and is circulated, and which operates with a distillate pressure of 35-350 mbar and a distillate temperature of 18.degree.-70.degree. C., with the esters of tetrahydropyran-4-carboxylic acid being removed between plates 8 and 18 at 90.degree.-150.degree. C., and, where appropriate,c) feeding the bottom product from the second column into a third column with 5-25 theoretical plates, and returning the overhead products at a distillate pressure of 1-100 mbar and a distillate temperature of 90.degree.-140.degree. C. to the synthesis of the esters of tetrahydropyran-4-carboxylic acid.

    摘要翻译： 用于纯化式I的四氢吡喃-4-羧酸的酯的方法，其中R 1至R 3各自为C 1 -C 4 - 烷基，R 2和R 3各自为氢， 其中R 2和R 3具有上述含义，R 4是氢，1-6个碳的烷基或式-CO-R 2的酰基，其中式R 1 OH的醇在存在下 氧化物催化剂，通过蒸馏，其需要a）在具有5-25理论塔板的第一塔中，馏出物压力为700-1100毫巴，馏出物温度为50-80℃，醇和升高 至10％的水，b）将底部产物从第一塔转移到具有18-40理论塔板的第二塔中，其中在15和30之间计量水夹带剂，并循环，并且其以 馏出液压力为35-350毫巴，馏出物温度为18-70℃， 其中四氢吡喃-4-羧酸的酯在90℃-150℃下在板8和18之间除去，并且在适当的情况下，c）将底部产物从第二塔进料到具有5-25理论值的第三塔 将塔顶馏出物返回到馏出物压力为1-100毫巴，馏出液温度为90-140℃，以合成四氢吡喃-4-羧酸酯。

    Preparation of 3-(2-acyloxyethyl)-dihydro-2(3H)furanones
    3.
    发明授权
    Preparation of 3-(2-acyloxyethyl)-dihydro-2(3H)furanones 失效
    3-（2-酰氧基乙基） - 二氢-2（3H）呋喃酮的制备

    公开(公告)号：US5466831A

    公开(公告)日：1995-11-14

    申请号：US99232

    申请日：1993-07-29

    申请人： Werner Schnurr ,  Rolf Fischer ,  Norbert Goetz ,  Thomas Kuekenhoehner

    发明人： Werner Schnurr ,  Rolf Fischer ,  Norbert Goetz ,  Thomas Kuekenhoehner

    IPC分类号： C07D307/33 ,  C07D307/12

    CPC分类号： C07D307/33

    摘要： A process for the preparation of 3-(2'-acyloxyethyl)-dihydro-2(3H)furanones of the general formula I ##STR1## in which R.sup.1 denotes C.sub.1 -C.sub.12 alkyl, C.sub.5 -C.sub.8 cycloalkyl, aryl, C.sub.7 -C.sub.12 aralkyl, or C.sub.7 -C.sub.12 alkylaryl, in which a 3-(2'-oxyethyl)-dihydro-2(3H)furanone of the general formula II ##STR2## in which R.sup.2 denotes C.sub.1 -C.sub.12 alkyl, C.sub.5 -C.sub.8 cycloalkyl, aryl, C.sub.7 -C.sub.12 aralkyl, or C.sub.7 -C.sub.12 alkylaryl is caused to react with a carboxylic acid, a carboxylic anhydride, and/or an acyl halide in the presence of an acid catalyst at temperatures of from 50.degree. to 250.degree. C. and pressures of from 0.1 to 100 bar.

    摘要翻译： 制备通式I，C5-C8环烷基，芳基，C7-C12芳烷基或C7-C12烷基芳基的3-（2'-酰氧基乙基） - 二氢-2（3H）呋喃酮的方法，其中3 - （2'-氧乙基） - 二氢-2（3H）呋喃酮，其中R 2表示C 1 -C 12烷基，C 5 -C 8环烷基，芳基，C 7 -C 12芳烷基或C 7 -C 12芳烷基， C12烷基芳基在酸催化剂存在下，在50-250℃，压力为0.1-100巴的条件下，与羧酸，羧酸酐和/或酰卤反应。

    Preparation of tetrahydropyran-4-carboxylic acid and esters thereof
    4.
    发明授权
    Preparation of tetrahydropyran-4-carboxylic acid and esters thereof 失效
    四氢吡喃-4-羧酸及其酯的制备

    公开(公告)号：US5371246A

    公开(公告)日：1994-12-06

    申请号：US110219

    申请日：1993-08-23

    申请人： Dirk Borchers ,  Rolf Fischer ,  Norbert Goetz ,  Thomas Kuekenhoehner ,  Werner Schnurr

    发明人： Dirk Borchers ,  Rolf Fischer ,  Norbert Goetz ,  Thomas Kuekenhoehner ,  Werner Schnurr

    IPC分类号： B01J21/04 ,  C07B61/00 ,  C07D309/08 ,  C07D309/06

    CPC分类号： C07D309/08

    摘要： A process for the preparation of tetrahydropyran-4-carboxylic acid and esters thereof of the general formula I ##STR1## in which R.sup.1 denotes hydrogen, C.sub.1 -C.sub.6 alkyl, C.sub.5 -C.sub.8 cycloalkyl, or aryl by the reaction of a dihydro-2(3H)furanone of the general formula II ##STR2## in which R.sup.2 denotes hydrogen, C.sub.1 -C.sub.6 alkyl, or --CO--R.sup.3 andR.sup.3 denotes hydrogen or C.sub.1 -C.sub.6 alkyl, with water or an alcohol of the general formula IIIR.sup.1 --OH (III),in whichR.sup.1 has the aforementioned meaning,at temperatures ranging from 200.degree. to 350.degree. C. in the presence of a heterogenous acid catalyst, in which use is made of a fixed heterogenous acid catalyst.

    摘要翻译： 制备通式I的四氢吡喃-4-羧酸及其酯的方法，其中R 1表示氢，C 1 -C 6烷基，C 5 -C 8环烷基或芳基，其中二氢 -2（3H）呋喃酮，其中R 2表示氢，C 1 -C 6烷基或-CO-R 3，R 3表示氢或C 1 -C 6烷基，其中R 2表示氢或C 1 -C 6烷基， 在异种酸催化剂的存在下，在200〜350℃的温度范围内，通式III的R1-OH（Ⅲ），其中R 1具有上述含义，其中使用固定的异种酸催化剂。

    Preparation of 3-(2'-oxyethyl)dihydro-2(3H)furanones
    5.
    发明授权
    Preparation of 3-(2'-oxyethyl)dihydro-2(3H)furanones 失效
    制备3-（2'-氧乙基）二氢-2（3H）呋喃酮

    公开(公告)号：US5350863A

    公开(公告)日：1994-09-27

    申请号：US120439

    申请日：1993-09-14

    申请人： Thomas Kuekenhoehner ,  Norbert Goetz ,  Rolf Fischer ,  Werner Schnurr ,  Dirk Borchers

    发明人： Thomas Kuekenhoehner ,  Norbert Goetz ,  Rolf Fischer ,  Werner Schnurr ,  Dirk Borchers

    IPC分类号： C07D307/33 ,  C07D307/20

    CPC分类号： C07D307/33

    摘要： A process for preparing 3-(2'-oxyethyl)dihydro-2(3H)furanones of the general formula I ##STR1## where R.sup.1 is hydrogen or acetyl, by reacting ethylene oxide with acetoacetic acid esters of the general formula II ##STR2## where R.sup.2 is C.sub.1 -C.sub.4 -alkyl, which comprises carrying out the reaction in alcoholic solutions in the presence of alkali metal alkoxides at from 20.degree. to 100.degree. C. and from 1 to 20 bar, is described.

    摘要翻译： 制备通式Ⅰ的3-（2'-氧乙基）二氢-2（3H）呋喃酮的方法，其中R1是氢或乙酰基，通过使环氧乙烷与通式II的乙酰乙酸酯反应 其中R 2是C 1 -C 4 - 烷基，其包括在20至100℃和1至20巴的碱金属醇盐存在下，在醇溶液中进行反应。

    Preparation of carboxylic esters
    6.
    发明授权
    Preparation of carboxylic esters 失效
    羧酸酯的制备

    公开(公告)号：US5412120A

    公开(公告)日：1995-05-02

    申请号：US158361

    申请日：1993-11-29

    申请人： Rolf Fischer ,  Norbert Goetz ,  Thomas Kuekenhoehner ,  Werner Schnurr

    发明人： Rolf Fischer ,  Norbert Goetz ,  Thomas Kuekenhoehner ,  Werner Schnurr

    IPC分类号： C07C67/475 ,  C07D309/08 ,  C07D315/00

    CPC分类号： C07C67/475 ,  C07D309/08

    摘要： A process for preparing monocarboxylic esters of the general formula I ##STR1## where R.sup.1 and R.sup.2 are each hydrogen, C.sub.1 -C.sub.12 -alkyl, C.sub.3 -C.sub.8 -cyclo-alkyl acyl, aryl or C.sub.7 -C.sub.20 -aralkyl or together --(CH.sub.2).sub.n --X--(CH.sub.2).sub.m --,X is methylene, oxygen, sulfur, NH or NR.sup.3,R.sup.3 is C.sub.1 -C.sub.12 -alkyl, andn and m are each from 0 to 8, comprises reacting geminal dicarboxylic esters of the general formula II ##STR2## where R.sup.1 to R.sup.3 are each as defined above, at from 150.degree. to 400.degree. C. in the presence of catalysts.

    摘要翻译： 一种制备通式I的单羧酸的方法，其中R 1和R 2各自为氢，C 1 -C 12 - 烷基，C 3 -C 8 - 环烷基酰基，芳基或C 7 -C 20 - 芳烷基或一起 - （CH 2 ）nX-（CH 2）m - ，X是亚甲基，氧，硫，NH或NR 3，R 3是C 1 -C 12烷基，n和m各自为0至8，包括使通式II的偕二羧酸酯 其中R 1至R 3各自如上所定义，在150℃至400℃下，在催化剂存在下。

    Preparation of .alpha.,.beta.-unsaturated carbonyl compounds
    9.
    发明授权
    Preparation of .alpha.,.beta.-unsaturated carbonyl compounds 失效
    （ALPHA），（BETA） - 饱和碳化合物的制备

    公开(公告)号：US5169958A

    公开(公告)日：1992-12-08

    申请号：US769022

    申请日：1991-10-01

    申请人： Heinz Isak ,  Norbert Goetz ,  Thomas Kuekenhoehner

    发明人： Heinz Isak ,  Norbert Goetz ,  Thomas Kuekenhoehner

    IPC分类号： C07C45/67 ,  C07C45/68 ,  C07C47/232 ,  C07C47/24 ,  C07C47/277 ,  C07C223/02 ,  C07C225/16 ,  C07C229/34

    CPC分类号： C07C229/34 ,  C07C223/02 ,  C07C225/16 ,  C07C45/673 ,  C07C45/68 ,  C07C47/232 ,  C07C47/24 ,  C07C47/277

    摘要： A process for the preparation of .alpha.,.beta.-unsaturated carbonyl compounds of the formula I ##STR1## where R.sup.1 is hydrogen, C.sub.1 -C.sub.10 -alkyl, C.sub.1 -C.sub.10 -alkoxy or aryloxy,R.sup.2 is aryl which is unsubstituted or substituted by C.sub.1 -C.sub.4 -alkyl, C.sub.1 -C.sub.4 -alkoxy, trifluoromethyl and/or halogen andR.sup.3 is tetrahydrofuranyl or aryl which is substituted by C.sub.1 -C.sub.4 -alkyl, C.sub.1 -C.sub.4 -alkoxy, trifluoromethyl and/or halogen, which comprises reacting 3-amino-2-propen-1-ones of the formula II ##STR2## where R.sup.1 and R.sup.2 have the abovementioned meanings, and R.sup.4 and R.sup.5 are, independently of one another, hydrogen, C.sub.1 -C.sub.10 -alkyl or aryl, with a magnesium halide of the formula IIIR.sup.3 --Mg--Y (III) where Y is halogen, at from -20.degree. to 100.degree. C., and novel .alpha.,.beta.-unsaturated carbonyl compounds and novel 3-amino-2-propen-1-ones are described.

    摘要翻译： 制备式I的α，β-不饱和羰基化合物的方法，其中R1是氢，C1-C10-烷基，C1-C10-烷氧基或芳氧基，R2是未取代或取代的芳基 C1-C4-烷基，C1-C4-烷氧基，三氟甲基和/或卤素，R3是被C1-C4-烷基，C1-C4-烷氧基，三氟甲基和/或卤素取代的四氢呋喃基或芳基，其包括使3 - 氨基-2-丙烯-1-酮，其中R 1和R 2具有上述含义，并且R 4和R 5彼此独立地为氢，C 1 -C 10 - 烷基或芳基， 与式III的卤化镁R3-Mg-Y（III）其中Y是卤素，在-20℃至100℃，和新的α，β-不饱和羰基化合物和新的3-氨基-2-丙烯 描述-1。