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    Purification of esters of tetrahydro-pyran-4-carboxylic acid
    32.
    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'-oxyethyl)dihydro-2(3H)furanones
    37.
    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。