公开(公告)号：US06346629B1

公开(公告)日：2002-02-12

申请号：US09700426

申请日：2000-11-15

申请人： Melanie Brunner ,  Ralf-Thomas Rahn ,  Udo Rheude ,  Jochem Henkelmann

发明人： Melanie Brunner ,  Ralf-Thomas Rahn ,  Udo Rheude ,  Jochem Henkelmann

IPC分类号： C07D30702

CPC分类号： C07D315/00

摘要： Process for producing butyrolactones of the general formula I where R1 and R2 are each hydrogen, alkyl, hydroxyalkyl, substituted or unsubstituted aryl or substituted or unsubstituted trialkylsilyl, by reacting alkynes of the general formula II where R1 and R2 are each as defined above, with carbon monoxide and water in the presence of a rhodium catalyst under pressures from 20 to 300 bar and hydrogenating the unhydrogenated 2(5H)-furanone intermediates comprises a) reacting the carbonylation reaction mixture with hydrogen at from 150 to 250° C. and from 100 to 300 bar, b) removing the precipitated catalyst and returning it into the carbonylation reaction, and c) subjecting the catalyst-free reaction mixture to a distillation to recover the butyrolactone.

摘要翻译： 制备通式I的丁内酯的方法，其中R 1和R 2各自为氢，烷基，羟基烷基，取代或未取代的芳基或取代或未取代的三烷基甲硅烷基，其中通式II的炔烃其中R 1和R 2各自如上所定义，与一氧化碳 和铑催化剂存在下的水，在20-300巴的压力下氢化未氢化的2（5H） - 呋喃酮中间体包括：a）使羰基化反应混合物与氢在150-250℃和100-300巴条件下反应 ，b）除去沉淀的催化剂并将其返回到羰基化反应中，和c）使无催化剂反应混合物进行蒸馏以回收丁内酯。

公开(公告)号：US06956141B1

公开(公告)日：2005-10-18

申请号：US09913979

申请日：2000-02-22

申请人： Melanie Maas-Brunner ,  Jochem Henkelmann ,  Gerd Kaibel ,  Alois Kindler ,  Christian Knoll ,  Harald Rust ,  Christian Tragut ,  Manfred Stroezel ,  Udo Rheude ,  Rudolf Erich Lorenz ,  Juan Aiscar

发明人： Melanie Maas-Brunner ,  Jochem Henkelmann ,  Gerd Kaibel ,  Alois Kindler ,  Christian Knoll ,  Harald Rust ,  Christian Tragut ,  Manfred Stroezel ,  Udo Rheude ,  Rudolf Erich Lorenz ,  Juan Aiscar

IPC分类号： C07C29/17 ,  C07C29/42 ,  C07C33/042 ,  C07C33/04 ,  C07C33/044 ,  C07C33/046

CPC分类号： C07C29/42 ,  C07C29/172 ,  Y02P20/582 ,  C07C33/044 ,  C07C33/042 ,  C07C31/20

摘要： A process for preparing at least one unsaturated alcohol (B) comprises the steps (I) to (III) below: (I) reaction of at least one alkali metal hydroxide or alkaline earth metal hydroxide with at least one alcohol (A) in at least one organic solvent (L) to give a mixture (G-I) comprising at least the alcohol (A), the solvent (L) and an alkoxide (AL); (II) reaction of at least one carbonyl compound of the formula R—CO—R′ with at least one alkyne of the formula R″—C≡C—H and the mixture (G-I) obtained in step (I) to give a mixture (G-II) comprising at least the alcohol (A), the solvent (L) and an unsaturated alcohol (B); (III) distillation of the mixture (G-II) obtained in step (II) to give the alcohol or alcohols (B) and a mixture (G-III) comprising the solvent (L) and the alcohol (A), wherein the solvent (L) obtained in step (III) and the alcohol (A) obtained in step (III) are recycled as a mixture to step (I).

摘要翻译： 一种制备至少一种不饱和醇（B）的方法包括下列步骤（I）至（III）：（I）至少一种碱金属氢氧化物或碱土金属氢氧化物与至少一种醇（A）在 至少一种有机溶剂（L），得到至少包含醇（A），溶剂（L）和醇盐（AL）的混合物（GI） （II）至少一种式R-CO-R'的羰基化合物与至少一种式R'-C≡CH的炔和步骤（I）中获得的混合物（GI）的反应，得到混合物 至少包含醇（A），溶剂（L）和不饱和醇（B）的化合物（G-II）; （II）中获得的混合物（G-II）的蒸馏（III），得到醇或醇（B）和包含溶剂（L）和醇（A）的混合物（G-III），其中 将步骤（III）中获得的溶剂（L）和步骤（III）中获得的醇（A）作为步骤（I）的混合物再循环。

公开(公告)号：US06054628A

公开(公告)日：2000-04-25

申请号：US955076

申请日：1997-10-21

申请人： Manfred Stroezel ,  Udo Rheude ,  Ralf-Thomas Rahn ,  Gerd Kaibel

发明人： Manfred Stroezel ,  Udo Rheude ,  Ralf-Thomas Rahn ,  Gerd Kaibel

IPC分类号： C07B49/00 ,  C07C29/124 ,  C07C29/40 ,  C07C31/00 ,  C07C33/02 ,  C07C35/18

CPC分类号： C07C29/40

摘要： In a process for carrying out an exothermal reaction, selected from the addition reaction of organomagnesium halide compounds to carbonyl compounds and the ensuing hydrolysis of the addition product, a considerable fraction of the heat liberated during the reaction is removed by evaporation of the solvent.

摘要翻译： 在进行放热反应的方法中，选自有机卤化镁化合物与羰基化合物的加成反应以及随后的加成产物的水解，通过蒸发溶剂除去反应期间释放出的相当大部分的热量。

公开(公告)号：US20100084257A1

公开(公告)日：2010-04-08

申请号：US12443563

申请日：2007-09-12

申请人： Helmut Schmidtke ,  Oliver Bussmann ,  Ralph Versch ,  Udo Rheude ,  Uwe Leyk ,  Manfred Julius ,  Martin Rudloff ,  Erhard Henkes

发明人： Helmut Schmidtke ,  Oliver Bussmann ,  Ralph Versch ,  Udo Rheude ,  Uwe Leyk ,  Manfred Julius ,  Martin Rudloff ,  Erhard Henkes

IPC分类号： C07C213/10 ,  C07D295/02 ,  B01D3/14 ,  C07C217/08

CPC分类号： C07D295/027

摘要： Processes for the continuous fractional distillation of a mixture comprising morpholine (MO), monoaminodiglycol (ADG), ammonia and water from a reaction of diethylene glycol (DEG) with ammonia, the process comprising: (i) separating off ammonia from the mixture at a top of a first distillation column K10; (ii) feeding a bottom fraction from K10 to a second distillation column K20 in which water and organic products are separated off at the top at a temperature at the top in the range from 45 to 198° C. and a pressure in the range from 0.1 to 15 bar, (iii) feeding a bottom fraction from K20 to a third distillation column K30, wherein the column K30 is a dividing wall column (DWC) which preferably has a dividing wall (DW) in the longitudinal direction of the column to form an upper combined column region (1), a lower combined column region (6), an inflow part (2, 4) having an enrichment section (2) and a stripping section (4), and also an offtake part (3, 5) having an enrichment section (3) and a stripping section (5), with the bottoms from K20 being fed in in the upper or middle third of the inflow part (2, 4), based on the number of theoretical plates of the inflow part, ADG and organic products having a boiling point of >190° C. (1.013 bar) being discharged at the bottom, organic products having a boiling point of ≦128° C. (1.013 bar) being discharged at the top and MO being discharged from the middle or lower third of the offtake part (3, 5) (side offtake), based on the number of theoretical plates of the offtake part.

摘要翻译： 用于从二甘醇（DEG）与氨的反应连续分馏含有吗啉（MO），单氨基二甘醇（ADG），氨和水的混合物的方法，该方法包括：（i）在 第一蒸馏塔K10顶部; （ii）将底部馏分从K10进料至第二蒸馏塔K20，其中水和有机产物在顶部分离出，顶部温度为45-98℃，压力范围为 0.1至15巴，（iii）从K20向第三蒸馏塔K30供给底部馏分，其中塔K30是分隔壁塔（DWC），其优选在塔的纵向方向上具有分隔壁（DW）至 形成上部组合列区域（1），下部组合列区域（6），具有浓缩部分（2）和剥离部分（4）的流入部分（2,4），以及出口部分（3， 5）具有富集部分（3）和汽提部分（5），其中来自K20的底部在流入部分（2,4）的上部或中部三分之一中被输入，基于理论塔板的数量 流入部件，ADG和沸点> 190℃（1.013巴）的有机产物在底部排出，有机原料 沸点为＆nlE; 128℃（1.013巴）在顶部排出，MO从出料部（3,5）的中部或下部三分之一（出口侧）排出，基于 理论板的出口部分。

公开(公告)号：US06541660B2

公开(公告)日：2003-04-01

申请号：US10106389

申请日：2002-03-27

申请人： Udo Rheude ,  Maximilian Vicari ,  Werner Aquila ,  Günter Wegner ,  Jörg Niekerken

发明人： Udo Rheude ,  Maximilian Vicari ,  Werner Aquila ,  Günter Wegner ,  Jörg Niekerken

IPC分类号： C07C6738

CPC分类号： C07C67/29 ,  C07C67/04 ,  C07C67/293 ,  C07C67/297 ,  C07C69/16 ,  C07C69/145

摘要： A process is proposed for preparing C5 acetate for Vitamin A synthesis by hydroformylation of 3,4-diacetoxybut-1-ene (3,4-DABE), according to which a 3,4-DABE is used which is obtained by acetoxylation of 1,3-butadiene with acetic acid and air in the presence of a catalyst and removing by distillation the 3,4-DABE formed in this case as by-product.

公开(公告)号：US06288282B1

公开(公告)日：2001-09-11

申请号：US09567268

申请日：2000-05-09

申请人： Udo Rheude ,  Ulrich Hörcher ,  Dietmar Weller ,  Manfred Stroezel

发明人： Udo Rheude ,  Ulrich Hörcher ,  Dietmar Weller ,  Manfred Stroezel

IPC分类号： C07C4921

CPC分类号： C07C403/16 ,  C07C2601/16

摘要： Process for the continuous preparation of &agr;- and/or &bgr;-ionone or homologous compounds using concentrated sulfuric acid at temperatures from 20 to 90° C., in the presence of organic solvents or diluents with cooling and by subsequent termination of the reaction by hydrolysis of the reaction mixture with water or dilute sulfuric acid, wherein both the cyclization of pseudoionones and the subsequent hydrolysis of the reaction mixture are carried out in a virtually adiabatic reaction in one or more reaction mixing pump(s) which are connected in series and each of which consists essentially of a rotationally symmetrical mixing chamber formed from a peripheral wall and two end walls and of a mixing rotor made of material inert to sulfuric acid and with rotational drive, where the mixing chamber has at least one inlet opening for each component and one outlet opening for the reaction mixture, and annular channels in fluid connection to one another in the end walls, and wherein the heat of the two reactions is in each case partly or wholly removed with the aid of a downstream heat exchanger.

摘要翻译： 使用浓硫酸在20〜90℃的温度下，在有机溶剂或稀释剂存在下，在冷却下，随后通过水解终止反应，连续制备α-和/或β-紫罗兰酮或同系化合物的方法 反应混合物与水或稀硫酸反应，其中假戊烯酮的环化和随后的反应混合物的水解在一个或多个反应混合泵中实质上绝热的反应中进行，所述反应混合泵串联连接， 其基本上由旋转对称的混合室组成，该混合室由周壁和两个端壁以及由硫酸惰性且具有旋转驱动的材料制成的混合转子，其中混合室具有用于每个部件的至少一个入口， 用于反应混合物的一个出口，以及在端壁中彼此流体连接的环形通道，其中热量 在每种情况下，两个反应在下游热交换器的帮助下部分或全部去除。

公开(公告)号：US08557985B2

公开(公告)日：2013-10-15

申请号：US13423956

申请日：2012-03-19

申请人： Bram Willem Hoffer ,  Hartwig Voβ ,  Ekkehard Schwab ,  Udo Rheude ,  Gerd Kaibel ,  Mathias Haake ,  Jan Eberhardt ,  Michael Karcher

发明人： Bram Willem Hoffer ,  Hartwig Voβ ,  Ekkehard Schwab ,  Udo Rheude ,  Gerd Kaibel ,  Mathias Haake ,  Jan Eberhardt ,  Michael Karcher

IPC分类号： C07D265/30 ,  C07C211/01 ,  C07C5/02

CPC分类号： C07C45/62 ,  C07C47/228 ,  C07C49/04 ,  C07C47/02

摘要： A process continuously hydrogenating unsaturated compounds, in which particles of a first hydrogenation catalyst are suspended in a liquid phase in which an unsaturated compound is dissolved, the liquid phase, in the presence of a hydrogenous gas at a first partial hydrogen pressure and at a first temperature, is conducted through a packed bubble column reactor in cocurrent counter to the direction of gravity, the effluent from the bubble column reactor is sent to a gas-liquid separation, the liquid phase is sent to a crossfiltration to obtain a retentate and a filtrate, the retentate is recycled into the bubble column reactor and the filtrate, in the presence of a hydrogenous gas at a second partial hydrogen pressure and at a second temperature, is passed over a bed of a second hydrogenation catalyst, the second partial hydrogen pressure is at least 10 bar higher than the first partial hydrogen pressure.

摘要翻译： 将第一氢化催化剂的颗粒悬浮在其中溶解有不饱和化合物的液相中的不饱和化合物的液相，在第一部分氢气压力下的氢气存在下的液相， 温度，通过与泡沫塔反应器并流反向并流并通过气泡塔反应器进行气液分离，将液相送至交叉过滤以获得滞留物和滤液 ，将渗余物再循环到泡罩塔反应器中，并且在第二部分氢气压力和第二温度下在氢气存在下将滤液通过第二氢化催化剂床，第二部分氢气压力为 比第一部分氢气压力高至少10巴。

公开(公告)号：US06300524B1

公开(公告)日：2001-10-09

申请号：US09440281

申请日：1999-11-15

申请人： Carsten Oost ,  Manfred Stroezel ,  Heinz Etzrodt ,  Dietmar Weller ,  Udo Rheude ,  Gerd Kaibel ,  Thomas Krug ,  Luise Spiske ,  Hagen Jaedicke

发明人： Carsten Oost ,  Manfred Stroezel ,  Heinz Etzrodt ,  Dietmar Weller ,  Udo Rheude ,  Gerd Kaibel ,  Thomas Krug ,  Luise Spiske ,  Hagen Jaedicke

IPC分类号： C07C4500

CPC分类号： C07C45/676 ,  Y02P20/582 ,  C07C49/255 ,  C07C49/203

摘要： The present invention relates to an improved process for preparing higher unsaturated ketones by reacting the corresponding &agr;,&bgr;-unsaturated alcohols with alkyl acetoacetates in a Carroll reaction , in a reactor system with fitted fractionation column, wherein A the &agr;,&bgr;-unsaturated alcohol is introduced into the reaction vessel together with the organic aluminum compound in the absence of effective amounts of a solvent, and the alkyl acetoacetate is metered into this mixture, B a reaction temperature which is as constant as possible at between 175° C. and 220° C., preferably between 180° C. and 200° C., is adjusted and C during the reaction the content of alkyl acetoacetate in the reaction mixture is adjusted to a value which is as constant as possible at between 1 and 3% by weight. It is advantageous in this process for the reaction temperature defined under B to be controlled by suitable variation of the heat input and/or by variation of the rate of addition of the alkyl acetoacetate, and for adequate mixing of the reaction mixture in the reaction vessel to be ensured This can be achieved with the aid of a stirrer, by pumping the reaction mixture through an external liquid circulation, by introducing the alkyl acetoacetate by means of a mixing nozzle or else by passing in a stream of inert gas. The process according to the invention is particularly suitable for the Carroll reaction of higher alcohols such as 3,7-dimethyl-1,6-octadien-3-ol (linalool), 3,7-dimethyl-1-octen-3-ol, 3,7,11-trimethyl-1,6,10-dodecatrien-3-ol (nerolidol), 3,7,11-trimethyl-1-dodecen-3-ol or 3,7,11-trimethyl-1,6-dodecadien-3-ol (dihydronerolidol).

摘要翻译： 本发明涉及一种改进的制备高级不饱和酮的方法，该方法通过在具有合适分馏塔的反应器系统中，在卡罗尔反应中使相应的α，β-不饱和醇与烷基乙酰乙酸酯反应，其中引入α，β-不饱和醇 在没有有效量的溶剂的情况下，将有机铝化合物与有机铝化合物一起加入到反应容器中，并将乙酰乙酸烷基酯计量加入到该混合物中，B在175℃和220℃之间的反应温度尽可能恒定 在反应过程中，优选在180℃和200℃之间调节和C，将反应混合物中乙酰乙酸烷基酯的含量调节至1至3重量％之间尽可能恒定的值。 在该方法中，通过适当变化的热输入和/或通过烷基的加成速率的变化来控制在B下限定的反应温度， 乙酰乙酸酯，并使反应混合物在反应容器中充分混合以确保这可以借助于搅拌器，通过泵送反应混合物通过外部液体循环，通过引入烷基乙酰乙酸酯通过混合喷嘴 或者通过流入惰性气体流。根据本发明的方法特别适用于高级醇如3,7-二甲基-1,6-辛二烯-3-醇（芳樟醇），3， 7,7-二甲基-1-辛烯-3-醇，3,7,11-三甲基-1,6,10-十二碳三烯-3-醇（橙花叔醇），3,7,11-三甲基-1-十二碳烯-3-醇 或3,7,11-三甲基-1,6-十二碳二烯-3-醇（二氢吗啉醇）。

公开(公告)号：US06211416B1

公开(公告)日：2001-04-03

申请号：US09424855

申请日：1999-12-06

申请人： Joaquim Henrique Teles ,  Norbert Rieber ,  Klaus Breuer ,  Dirk Demuth ,  Hartmut Hibst ,  Heinz Etzrodt ,  Udo Rheude

发明人： Joaquim Henrique Teles ,  Norbert Rieber ,  Klaus Breuer ,  Dirk Demuth ,  Hartmut Hibst ,  Heinz Etzrodt ,  Udo Rheude

IPC分类号： C07C4128

CPC分类号： C07C41/08 ,  C07C41/28 ,  C07C41/54 ,  C07C43/303 ,  C07C43/16 ,  C07C43/15

摘要： Enol ethers of the formula I where R1 is an aliphatic, cycloaliphatic, araliphatic, aromatic or heterocyclic radical which may carry further substituents which do not react with acetylenes or allenes, and the radicals R, independently of one another, are hydrogen or aliphatic, cycloaliphatic, araliphatic, aromatic or heterocyclic radicals, which may be bonded to one another to form a ring, and m is 0 or 1, are prepared by reacting an acetal or ketal of the formula II with an acetylene or allene of the formula III or IV where R and R1 have the abovementioned meanings, in the gas phase at elevated temperatures in the presence of a zinc- or cadmium- and silicon- and oxygen-containing heterogeneous catalyst.

摘要翻译： 式I的烯醇醚，其中R 1是脂族，脂环族，芳脂族，芳族或杂环基团，其可以进一步携带不与炔或全烯反应的取代基，并且基团R彼此独立地为氢或脂族，脂环族， 芳族或芳族杂环基，其可以彼此结合形成环，并且m为0或1，通过使式II的缩醛或缩酮与式III或IV的炔或丙烯的反应来制备，其中R和 R1在具有锌或镉和含硅和含氧异相催化剂存在下的高温下在气相中具有上述含义。

公开(公告)号：US5356636A

公开(公告)日：1994-10-18

申请号：US991318

申请日：1992-12-16

申请人： Joachim U. Schneider ,  Horst Schumacher ,  Wolfgang Bewert ,  Guenter Gaus ,  Udo Rheude

发明人： Joachim U. Schneider ,  Horst Schumacher ,  Wolfgang Bewert ,  Guenter Gaus ,  Udo Rheude

IPC分类号： A61K9/14 ,  A61K9/16 ,  A61K9/50 ,  A61K31/015 ,  A61K47/18 ,  A61K47/42 ,  A61P3/02

CPC分类号： A61K9/1623 ,  A61K9/1658

摘要： A process for preparing stable dry powders which are insoluble in hot water and which contain fat-soluble vitamins and/or carotenoids, which comprises the following steps:a) preparing an aqueous dispersion containing essentially these fat-soluble active substances, film-forming colloids and reducing sugars,b) converting this dispersion into dry vitamin and/or carotenoid products in powder form andc) thermally curing the powder at from 60.degree. to 180.degree. C.,wherein gelatin in combination with one or more organic amino compounds which are free or bonded in the manner of a salt and which contain a basic primary amino group and, in addition, either another amino group, a hydroxyl group, an alkoxy group or a carboxyl group, and/or in combination with sufficient basic alkali metal or alkaline earth metal compound for the dispersion to have a pH of from 7.5 to 10, is used as film-forming colloid, and the dry powders obtainable via this process are described.

摘要翻译： 一种制备不溶于热水并含有脂溶性维生素和/或类胡萝卜素的稳定干粉的方法，包括以下步骤：a）制备基本上含有这些脂溶性活性物质的成膜胶体，成膜胶体 和还原糖，b）将该分散体转化成粉末形式的干燥维生素和/或类胡萝卜素产品，和c）在60℃至180℃下热处理该粉末，其中明胶与一种或多种有机氨基化合物组合， 以盐的方式游离或键合，并含有碱性伯氨基，另外氨基，羟基，烷氧基或羧基，和/或与足够碱性碱金属或 使用pH7.5〜10的分散液的碱土金属化合物作为成膜胶体，对通过该方法得到的干粉进行说明。