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    • 127. 发明授权
    • Preparation of 3-(hydroxyphenyl)propionaldehydes and their hydrogenation
to 3-(hydroxyphenyl)propanols
    • 3-(羟基苯基)丙醛的制备及其氢化为3-(羟基苯基)丙醇
    • US5304685A
    • 1994-04-19
    • US037881
    • 1993-03-26
    • Franz MergerMartin Schmidt-Radde
    • Franz MergerMartin Schmidt-Radde
    • C07B61/00C07C37/00C07C39/11C07C45/68C07C45/71C07C47/27C07C45/00C07C29/14
    • C07C39/11C07C45/71C07C47/27
    • A process for preparing 3-(hydroxyphenyl)propionaldehydes of the formula I ##STR1## and, where appropriate, for preparing 3-(hydroxyphenyl)propanols of the formula II ##STR2## where R.sup.1, R.sup.2, R.sup.3 and R.sup.4 are each hydrogen, C.sub.1 -C.sub.20 -alkyl, C.sub.3 -C.sub.20 -cycloalkyl, C.sub.4 -C.sub.20 -alkylcycloalkyl, C.sub.4 -C.sub.20 -cycloalkylalkyl or C.sub.5 -C.sub.20 -alkylcycloalkylalkyl,R.sup.3 and R.sup.4 are each aryl, C.sub.7 -C.sub.20 -aralkyl, heterocycloalkyl or C.sub.3 -C.sub.20 -heterocycloalkylalkyl, entailsa) reacting phenols of the formula III ##STR3## where R.sup.1 and R.sup.2 have the abovementioned meanings, with 3-hydroxypropionaldehydes of the formula IV ##STR4## where R.sup.3 and R.sup.4 have the abovementioned meanings, in the presence of a basic catalyst at from 90.degree. to 230.degree. C. and under from 0.01 to 50 bar and, where appropriate,b) treating the resulting 3-(hydroxyphenyl)propionaldehydes of the formula I ##STR5## where R.sup.1, R.sup.2, R.sup.3 and R.sup.4 have the abovementioned meanings, with hydrogen in the presence of a hydrogenation catalyst at from 0.degree. to 250.degree. C. and under from 0.1 to 300 bar.
    • 制备式I(I)的3-(羟基苯基)丙醛的方法,以及适当时制备式II的3-(羟基苯基)丙醇的方法,其中R 1,R 2,R 3和 R 4各自为氢,C 1 -C 20 - 烷基,C 3 -C 20 - 环烷基,C 4 -C 20 - 烷基环烷基,C 4 -C 20 - 环烷基烷基或C 5 -C 20 - 烷基环烷基烷基,R 3和R 4各自为芳基,C 7 -C 20 - 芳烷基,杂环烷基或 C 3 -C 20杂环烷基烷基需要a)使具有上述含义的式III化合物III(III)的酚与式IV的3-羟基丙醛反应,其中R 3和R 4具有 在碱性催化剂存在下,在90〜230℃,0.01〜50巴下,适当时,b)处理得到的式(I)的3-(羟基苯基)丙醛 I)其中R 1,R 2,R 3和R 4具有上述含义,在氢化催化剂存在下,在0〜250℃下, 0.1至300巴。
    • 128. 发明授权
    • Recovery of trialkylamines and methyl formate from mixtures obtained in
the preparation of trimethylolalkanes
    • 三氯甲烷制备中获得的混合物中的丙烯酰胺和甲基丙烯酸的回收
    • US5149861A
    • 1992-09-22
    • US664463
    • 1991-03-01
    • Franz MergerPeter HettingerLeopold HupferJuergen PaetschHeribert DeckHeinz AuerErwin Brunner
    • Franz MergerPeter HettingerLeopold HupferJuergen PaetschHeribert DeckHeinz AuerErwin Brunner
    • C07C69/06C07C27/00C07C27/02C07C29/38C07C29/74C07C29/88C07C31/22C07C67/00C07C67/03C07C67/08C07C209/00C07C209/86C07C211/03C07C211/05
    • C07C29/88C07C67/03
    • Trialkylamines and methyl formate are recovered from reaction mixtures obtained in the preparation of trimethylolalkanes by reaction of n-alkanals with from 2.2 to 4.5 moles of formaldehyde in aqueous solution in the presence of from 0.6 to 3 mole of trialkylamine, each quantity based on 1 mole of alkanal, and subsequent hydrogenation in a process wherein the crude reaction mixturea) is heated to from 100.degree. to 200.degree. C., the water present in the reaction mixture is substantially separated off by distillation, together with any excess free trialkylamine, the trialkylamine present in the form of a trialkylammonium formate is freed to form a trimethylolalkane formate, the trialkylamine is distilled off and the trimethylolalkane formate is transesterified with methanol to trimethylolalkane and methyl formate in the presence or absence of a catalytic amount of an alkali metal alkoxide or alkaline earth metal alkoxide, orb) is substantially dewatered, any excess free trialkylamine being removed at the same time, the trialkylamine present in the form of a trialkylammonium formate is separated off by admixing the remaining mixture with methanol and heating the admixture to from 100.degree. to 200.degree. C. to form methyl formate and trialkylamine.
    • 三烷基胺和甲酸甲酯从制备三羟甲基烷烃得到的反应混合物中回收,通过在0.6至3摩尔三烷基胺存在的情况下,正链烷与2.2至4.5摩尔甲醛在水溶液中的反应,每个量基于1摩尔 然后在将粗反应混合物a)加热至100至200℃的过程中随后进行氢化,反应混合物中存在的水通过蒸馏与任何过量的游离三烷基胺基本上分离出来, 以三烷基铵甲酸盐形式存在的三烷基胺可以形成甲酸三羟甲基烷烃,在存在或不存在催化量的碱金属醇盐的条件下,将三烷基胺蒸馏除去,甲醇三甲氧基链烷烃甲酯与甲醇酯交换为三羟甲基烷烃和甲酸甲酯,或 碱土金属醇盐或b)基本脱水,任何过量游离的三烷基胺为 同时除去以三烷基甲酸铵形式存在的三烷基胺,通过将剩余的混合物与甲醇混合并将混合物加热至100至200℃以分离,形成甲酸甲酯和三烷基胺。
    • 130. 发明授权
    • Conversion of 1,3-dioxanes to 4-oxaaldehydes
    • 1,3-二恶烷转化为4-氧杂醛
    • US5012005A
    • 1991-04-30
    • US385925
    • 1989-07-27
    • Wolfgang HoelderichFranz Merger
    • Wolfgang HoelderichFranz Merger
    • C07C45/60C07C47/198C07C47/277C07D335/02
    • C07C47/277C07C45/60C07C47/198C07D335/02
    • 4-oxaaldehydes of the formula ##STR1## are prepared by catalytic isomerization of 1,3-dioxanes by a process in which a 1,3-dioxane of the formula ##STR2## where R.sup.1, R.sup.2, R.sup.4 and R.sup.5 are identical or different and are each hydrogen, a straight-chain or branched alkyl, alkenyl or alkynyl radical of not more than 18 carbon atoms, a cycloalkyl or cycloalkenyl radical of 5 to 8 carbon atoms, an aryl, alkylaryl, aralkyl, aralkenyl or alkenylaryl radical of 5 to 16 carbon atoms or a heterocyclic radical and furthermore R.sup.1 and R.sup.2 and/or R.sup.4 and R.sup.5 together with the carbon atoms to which they are bonded may form a cycloalkane, a cycloalkene or a heterocyclic structure, and the stated radicals may furthermore carry substituents which are inert under the reaction conditions, and R.sup.3 is hydrogen or straight-chain or branched alkyl, is isomerized using a metal oxide catalyst, which has been treated with an acid, and/or a silica phase having a zeolite structure.
    • 通过其中R1,R2,R4和R5是相同或不同的式“IMAGE”的1,3-二恶烷的方法,通过1,3-二恶烷的催化异构化制备式“IMAGE”的4-氧代醛, 各自为氢,不超过18个碳原子的直链或支链烷基,烯基或炔基,5至8个碳原子的环烷基或环烯基,芳基,烷基芳基,芳烷基,芳烯基或链烯基芳基,其5至 16个碳原子或杂环基团,此外,R 1和R 2和/或R 4和R 5与它们所键合的碳原子一起可以形成环烷烃,环烯烃或杂环结构,并且所述基团还可以具有取代基, 使用已用酸处理的金属氧化物催化剂和/或具有沸石结构的二氧化硅相异构化在反应条件下惰性的R 3为氢或直链或支链烷基。