Purification of esters of tetrahydro-pyran-4-carboxylic acid
    4.
    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

    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。

    Isoxazole(isothiazole)-5-carboxamides
    9.
    发明授权
    Isoxazole(isothiazole)-5-carboxamides 失效
    异佛唑(异噻唑)-5-羧酰胺

    公开(公告)号:US5080708A

    公开(公告)日:1992-01-14

    申请号:US337640

    申请日:1989-04-13

    摘要: Isoxazole(isothiazole)-5-carboxamides of the formula ##STR1## where X is oxygen or sulfur,R.sup.1 is hydrogen, substituted or unsubstituted alkyl, alkoxy, substituted or unsubstituted cycloalkyl, a 5- or 6-membered heterocyclic radical having one or two heteroatoms selected from the group consisting of oxygen, sulfur and nitrogen, and which may be substituted, or substituted or unsubstituted phenyl, orR.sup.2 is formyl, 4,5-dihydrooxazol-2-yl or a radical of the formula COYR.sup.5 or CONR.sup.6 R.sup.7, whereY is oxygen or sulfur,R.sup.5 ishydrogen, substituted or unsubstituted alkyl, substituted or unsubstituted alkenyl, haloalkenyl, substituted or unsubstituted alkynyl,cycloalkyl,cycloalkenyl,substituted or unsubstituted phenyl,a 5- or 6-membered heterocyclic radical having one or two heteroatoms selected from the group consisting of oxygen, sulfur and nitrogen,cycloalkanimino, phthalimido, succinimido, or a radical ##STR2## R.sup.3 and R.sup.4 have the meanings defined herein, or their agriculturally acceptable salts possess herbicidal activity.

    摘要翻译: 其中X是氧或硫,R 1是氢,取代或未取代的烷基,烷氧基,取代或未取代的环烷基,具有一个或两个的5-或6-元杂环基的异噻唑(异噻唑)-5-甲酰胺, 选自氧,硫和氮的杂原子,并且其可以被取代,或取代或未取代的苯基,或R 2是甲酰基,4,5-二氢恶唑-2-基或式COYR 5或CONR 6 R 7的基团,其中 Y是氧或硫,R5是氢,取代或未取代的烷基,取代或未取代的烯基,卤代烯基,取代或未取代的炔基,环烷基,环烯基,取代或未取代的苯基,具有一个或两个杂原子的5-或6-元杂环基 选自氧,硫和氮,环亚烷基亚氨基,邻苯二甲酰亚氨基,琥珀酰亚胺基或自由基,CH 2 CH(OH)CH 2(OH)等,R 3和R 4具有本文定义的含义或其农业 超可接受的盐具有除草活性。