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    • 1. 发明授权
    • Purification of esters of tetrahydro-pyran-4-carboxylic acid
    • 四氢 - 吡喃-4-羧酸酯的纯化
    • US5414097A
    • 1995-05-09
    • US185179
    • 1994-01-24
    • Rolf FischerNorbert GoetzThomas KuekenhoehnerHarald RustWerner Schnurr
    • Rolf FischerNorbert GoetzThomas KuekenhoehnerHarald RustWerner Schnurr
    • C07D309/08
    • C07D309/08
    • 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.
    • 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。
    • 10. 发明授权
    • Preparation of aliphatic alpha omega-aminonitriles
    • 脂肪族α-ω-氨基腈的制备
    • US5801268A
    • 1998-09-01
    • US846240
    • 1997-04-28
    • Klemens FlickJohann-Peter MelderWerner SchnurrKlaus EbelTom WitzelWolfgang HarderAlwin RehfingerRolf Fischer
    • Klemens FlickJohann-Peter MelderWerner SchnurrKlaus EbelTom WitzelWolfgang HarderAlwin RehfingerRolf Fischer
    • B01J23/76B01J23/78B01J23/889B01J37/02C07C253/30C07C255/24C07C255/03
    • B01J23/76B01J23/78B01J23/8892B01J23/8898B01J37/0201C07C253/30
    • 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.
    • 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)。