Preparation of tetrahydropyran-4-carboxylic acid and esters thereof
    1.
    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

    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
    2.
    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

    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。

    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。

    Preparation of 3-(2-acyloxyethyl)-dihydro-2(3H)furanones
    5.
    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

    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 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

    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 aliphatic alpha omega-aminonitriles
    10.
    发明授权
    Preparation of aliphatic alpha omega-aminonitriles 失效
    脂肪族α-ω-氨基腈的制备

    公开(公告)号:US5801268A

    公开(公告)日:1998-09-01

    申请号:US846240

    申请日:1997-04-28

    摘要: Aliphatic alpha,omega-aminonitriles are prepared by partial hydrogenation of aliphatic alpha,omega-dinitriles at elevated temperatures and superatmospheric pressure in the presence of a solvent and of a catalyst by a process which comprises using a catalyst which (a) contains a compound based on a metal selected from the group consisting of nickel, cobalt, iron, ruthenium and rhodium and (b) contains from 0.01 to 25% by weight, based on (a), of a promoter based on a metal selected from the group consisting of palladium, platinum, iridium, osmium, copper, silver, gold, chromium, molybdenum, tungsten, manganese, rhenium, zinc, cadmium, lead, aluminum, tin, phosphorus, arsenic, antimony, bismuth and rare earth metals and (c) from 0 to 5% by weight, based on (a), of a compound based on an alkali metal or on an alkaline earth metal, with the proviso that the component (a) is not based on iron or iron and one of the metals selected from the group consisting of cobalt, ruthenium and rhodium when (b) is a promoter based on a metal selected from the group consisting of titanium, manganese, chromium and molybdenum, and with the further proviso that, when a compound based on only ruthenium or rhodium or ruthenium and rhodium or nickel and rhodium is selected as component (a), the promoter (b) may be dispensed with.

    摘要翻译: 脂肪族α,ω-氨基腈通过脂肪族α,ω-二腈在升高的温度和超大气压下,在溶剂和催化剂存在下通过包括使用(a)含有基于化合物的催化剂 在选自镍,钴,铁,钌和铑的金属上,和(b)含有基于(a)0.01至25重量%的基于选自以下的金属的促进剂: 钯,铂,铱,锇,铜,银,金,铬,钼,钨,锰,铼,锌,镉,铅,铝,锡,磷,砷,锑,铋和稀土金属和(c) 基于(a),基于碱金属或碱土金属的化合物为0至5重量%,条件是组分(a)不以铁或铁为基准,并且所选择的金属之一 来自由钴,钌和铑组成的组 母体(b)是基于选自钛,锰,铬和钼的金属的促进剂,进一步的条件是当仅基于钌或铑或钌和铑或镍和铑的化合物为 作为组分(a)选择,可以不用启动子(b)。