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公开(公告)号：US10669222B2
公开(公告)日：2020-06-02
申请号：US16338633
申请日：2017-10-05
申请人： BASF SE
发明人： Sebastian Wloch , Gunnar Heydrich , Matthias Rauls
摘要： The present invention relates to a process for enriching enantiomers from an enantiomer mixture by a fractionating melt crystallization in a melt crystallization apparatus. The invention specifically relates to a process for producing an enantiomer-enriched chiral terpene, in particular of D/L-Isopulegol. The process comprises: i) a crystallization step to obtain a crystallizate and a mother melt and removal of the mother melt from the crystallizate to afford a mother melt fraction; ii) sweating of the crystallizate obtained in step i) to afford a molten sweating fraction and iii) subsequent melting of the sweated crystallizate to afford a molten crystallizate fraction, wherein the optical rotation at least of the sweating fraction is determined online using a polarimeter and the changeover from step ii) to step iii) is controlled online by means of at least one control unit.
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公开(公告)号：US09975837B2
公开(公告)日：2018-05-22
申请号：US15536524
申请日：2015-12-18
申请人： BASF SE
发明人： Mathias Schelwies , Rocco Paciello , Gunnar Heydrich , Günter Wegner , Gerd-Dieter Tebben , Martin Haubner , Andreas Keller , Oliver Bey , Stephanie Renz , Georg Seeber
CPC分类号： C07C45/62 , C07B2200/07 , C07C29/172 , C07C29/56 , C07C2601/14 , C07C47/21 , C07C47/02 , C07C35/12 , C07C35/17
摘要： The present invention relates to a process for the preparation of an optically active carbonyl compound by asymmetric hydrogenation of a prochiral α,β-unsaturated carbonyl compound with hydrogen in the presence of at least one optically active transition metal catalyst that is soluble in the reaction mixture and which has rhodium as catalytically active transition metal and a chiral, bidentate bisphosphine ligand, wherein the reaction mixture during the hydrogenation of the prochiral α,β-unsaturated carbonyl compound additionally comprises at least one compound of the general formula (I): in which R1, R2: are identical or different and are C6- to C10-aryl which is unsubstituted or carries one or more, e.g. 1, 2, 3, 4 or 5, substituents which are selected from C1- to C6-alkyl, C3- to C6-cycloalkyl, C6- to C10-aryl, C1- to C6-alkoxy and amino; Z is a group CHR3R4 or aryl which is unsubstituted or carries one or more, e.g. 1, 2, 3, 4 or 5, substituents which are selected from C1- to C6-alkyl, C3- to C6-cycloalkyl, C6- to C10-aryl, C1- to C6-alkoxy and amino, wherein R3 and R4 are as defined in the claims and the description.
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3.发明申请公开(公告)号：US20140158515A1
公开(公告)日：2014-06-12
申请号：US13790465
申请日：2013-03-08
申请人： BASF SE
CPC分类号： B01D3/141 , B01D3/14 , C07B2200/07 , C07C29/80 , C07C2601/14 , C07C35/12 , C07C35/17
摘要： The present invention relates to a continuous process for preparing racemic or optically active menthol in pure or enriched form by distillatively separating menthol from substance mixtures which comprise essentially menthol and diastereomers thereof. This distillative separation is performed in a dividing wall column with 50 to 300 theoretical plates and one or more side draw points at an absolute operating pressure of 5 to 500 mbar.
摘要翻译： 本发明涉及通过将薄荷醇与基本上含有薄荷醇和非对映异构体的物质混合物蒸馏分离来制备纯的或富集形式的外消旋或光学活性薄荷醇的连续方法。 该蒸馏分离在具有50至300个理论塔板和一个或多个侧向牵引点的分隔壁塔中进行，其绝对操作压力为5至500毫巴。
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4.发明授权公开(公告)号：US11884611B2
公开(公告)日：2024-01-30
申请号：US17274135
申请日：2019-09-03
申请人： BASF SE
发明人： Oliver Bey , Peter Zehner , Michael Acker , Rocco Paciello , Mathias Schelwies , Martin Haubner , Guenter Wegner , Gerd Tebben , Gunnar Heydrich , Georg Seeber
IPC分类号： C07C29/141 , B01J10/00 , B01J3/04 , B01J19/00 , B01J19/24 , B01J19/26 , B01J19/30 , B01J19/32 , B01J31/20
CPC分类号： C07C29/141 , B01J3/042 , B01J10/00 , B01J10/002 , B01J19/0066 , B01J19/244 , B01J19/2465 , B01J19/26 , B01J19/30 , B01J19/32 , B01J31/20 , B01J2219/0009 , B01J2219/0025 , B01J2219/00092 , B01J2219/00096 , B01J2219/185 , B01J2219/1943 , B01J2531/822 , C07B2200/07
摘要： A reactor for performing a gas/liquid biphasic high-pressure reaction with a foaming medium, comprising an interior formed by a cylindrical, vertically oriented elongate shell, a bottom and a cap, wherein the interior is divided by internals into a backmixed zone and a zone of limited backmixing, wherein the backmixed zone and the zone of limited backmixing are consecutively traversable by the reaction mixture, wherein the backmixed zone comprises means for introducing gas and liquid and a gas outlet and also comprises at least one mixing apparatus selected from a stirrer, a jet nozzle and means for injecting the gas, and the zone of limited backmixing comprises a reaction product outlet, a first cylindrical internal element which in the interior extends in the longitudinal direction of the reactor and which delimits the zone of limited backmixing from the backmixed zone, backmixing-preventing second internal elements in the form of random packings, structured packings or liquid-permeable trays arranged in the zone of limited backmixing and a riser tube whose lower end is arranged within the backmixed zone and whose upper end opens into the zone of limited backmixing so that liquid from the backmixed zone can ascend into the zone of limited backmixing via the riser tube, wherein flow into the zone of limited backmixing enters from below. The reactor is configured such that the high-pressure reaction space is optimally utilized and contamination of workup steps or subsequent reactions arranged downstream of the high-pressure reaction with foam is substantially avoided. The invention further relates to a process for performing a continuous gas/liquid biphasic high-pressure reaction in the reactor.
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5.发明授权公开(公告)号：US11529607B2
公开(公告)日：2022-12-20
申请号：US17274148
申请日：2019-09-03
申请人： BASF SE
发明人： Oliver Bey , Peter Zehner , Mathias Schelwies , Rocco Paciello , Martin Haubner , Guenter Wegner , Gerd Tebben , Gunnar Heydrich , Georg Seeber , Michael Acker
摘要： A reactor for performing a reaction between two immiscible fluids of different density, comprising an interior formed by a cylindrical, vertically oriented elongate shell, a bottom and a cap, wherein the interior is divided by internals into a backmixed zone, a zone of limited backmixing preferably arranged below the backmixed zone and a plug-flow zone which are at least consecutively traversable by one of the fluids, wherein the backmixed zone comprises at least one inlet and the plug-flow zone comprises an outlet and the backmixed zone comprises at least one mixing apparatus selected from a stirrer, a jet nozzle and means for injecting the fluid of lower density, a first cylindrical internal element which in the interior extends in the longitudinal direction of the reactor, which delimits the zone of limited backmixing from the plug-flow zone and which comprises a first passage to the backmixed zone and a second passage to the plug-flow zone, a second internal element which delimits the backmixed zone from the plug-flow zone such that there is no direct fluid connection between the backmixed zone and the plug-flow zone, and backmixing-preventing third internal elements in the form of random packings, structured packings or liquid-permeable trays arranged in the zone of limited backmixing. The reactor allows an optimal residence time distribution in the reaction of the two immiscible fluids of different density. The invention further relates to a process for performing a continuous reaction in the reactor.
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公开(公告)号：US11766653B2
公开(公告)日：2023-09-26
申请号：US17274110
申请日：2019-09-03
申请人： BASF SE
发明人： Oliver Bey , Peter Zehner , Andreas Keller , Stephanie Renz , Mathias Schelwies , Rocco Paciello , Martin Haubner , Guenter Wegner , Gerd Tebben , Gunnar Heydrich , Georg Seeber
CPC分类号： B01J10/002 , B01J3/02 , B01J3/042 , B01J4/002 , B01J31/2409 , C07C45/62 , B01J2203/065 , B01J2531/822 , C07B53/00
摘要： A process for performing a continuous gas/liquid biphasic high-pressure reaction, wherein a gas and a liquid are introduced into a backmixed zone of a reactor and in the backmixed zone the gas is dispersed in the liquid by stirring, injection of gas and/or a liquid jet, a reaction mixture consecutively traverses the backmixed zone and a zone of limited backmixing, and a liquid reaction product is withdrawn at a reaction product outlet of the zone of limited backmixing, wherein the reactor comprises: an interior formed by a cylindrical vertically oriented elongate shell, a bottom and a cap, wherein the interior is divided by means of internals into the backmixed zone, the zone of limited backmixing and a cavity, a first cylindrical internal element which in the interior extends in the longitudinal direction of the reactor and which delimits the zone of limited backmixing from the backmixed zone, backmixing-preventing second internal elements in the form of random packings, structured packings or liquid-permeable trays arranged in the zone of limited backmixing and a third internal element which in the interior extends in the longitudinal direction of the reactor and is open at the bottom, wherein the third internal element forms the cavity in which gas bubbles collect and do not escape upwards, thus preventing the volume of the cavity from being occupied by liquid and reducing the reaction volume. The reaction volume of the reactor used in the process can be reversibly reduced in simple fashion. The invention further relates to a process for adapting the reaction volume of a reactor suitable for performing a gas/liquid biphasic high-pressure reaction having an outlet for a liquid reaction product in which an internal element is arranged so as to form a cavity open at the bottom in which gas bubbles collect and do not escape upwards, thus preventing the volume of the cavity from being occupied by liquid and reducing the reaction volume.
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公开(公告)号：USRE49036E1
公开(公告)日：2022-04-19
申请号：US16521935
申请日：2019-07-25
申请人： BASF SE
发明人： Mathias Schelwies , Rocco Paciello , Gunnar Heydrich , Günter Wegner , Gerd-Dieter Tebben , Martin Haubner , Andreas Keller , Oliver Bey , Stephanie Renz , Georg Seeber
摘要： The present invention relates to a process for the preparation of an optically active carbonyl compound by asymmetric hydrogenation of a prochiral α,β-unsaturated carbonyl compound with hydrogen in the presence of at least one optically active transition metal catalyst that is soluble in the reaction mixture and which has rhodium as catalytically active transition metal and a chiral, bidentate bisphosphine ligand, wherein the reaction mixture during the hydrogenation of the prochiral α,β-unsaturated carbonyl compound additionally comprises at least one compound of the general formula (I): in which R1, R2: are identical or different and are C6- to C10-aryl which is unsubstituted or carries one or more, e.g. 1, 2, 3, 4 or 5, substituents which are selected from C1- to C6-alkyl, C3- to C6-cycloalkyl, C6- to C10-aryl, C1- to C6-alkoxy and amino; Z is a group CHR3R4 or aryl which is unsubstituted or carries one or more, e.g. 1, 2, 3, 4 or 5, substituents which are selected from C1- to C6-alkyl, C3- to C6-cycloalkyl, C6- to C10-aryl, C1- to C6-alkoxy and amino, wherein R3 and R4 are as defined in the claims and the description.
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公开(公告)号：US10301244B2
公开(公告)日：2019-05-28
申请号：US15964400
申请日：2018-04-27
申请人： BASF SE
发明人： Mathias Schelwies , Rocco Paciello , Gunnar Heydrich , Günter Wegner , Gerd-Dieter Tebben , Martin Haubner , Andreas Keller , Oliver Bey , Stephanie Renz , Georg Seeber
摘要： The present invention relates to a process for the preparation of an optically active carbonyl compound by asymmetric hydrogenation of a prochiral α,β-unsaturated carbonyl compound with hydrogen in the presence of at least one optically active transition metal catalyst that is soluble in the reaction mixture and which has rhodium as catalytically active transition metal and a chiral, bidentate bisphosphine ligand, wherein the reaction mixture during the hydrogenation of the prochiral α,β-unsaturated carbonyl compound additionally comprises at least one compound of the general formula (I): in which R1, R2: are identical or different and are C6- to C10-aryl which is unsubstituted or carries one or more, e.g. 1, 2, 3, 4 or 5, substituents which are selected from C1- to C6-alkyl, C3- to C6-cycloalkyl, C6- to C10-aryl, C1- to C6-alkoxy and amino; Z is a group CHR3R4 or aryl which is unsubstituted or carries one or more, e.g. 1, 2, 3, 4 or 5, substituents which are selected from C1- to C6-alkyl, C3- to C6-cycloalkyl, C6- to C10-aryl, C1- to C6-alkoxy and amino, wherein R3 and R4 are as defined in the claims and the description.
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公开(公告)号：US09988331B2
公开(公告)日：2018-06-05
申请号：US13658003
申请日：2012-10-23
申请人： BASF SE
发明人： Gunnar Heydrich , Gabriele Gralla , Matthias Rauls , Joachim Schmidt-Leithoff , Klaus Ebel , Wolfgang Krause , Steffen Oehlenschläger , Christoph Jäkel , Marko Friedrich , Eike Johannes Bergner , Nawid Kashani-Shirazi , Rocco Paciello
CPC分类号： C07C29/56 , C07B2200/07 , C07C29/172 , C07C29/78 , C07C45/62 , C07C45/82 , C07C2601/14 , C07C2601/16 , C07C47/21 , C07C35/12 , C07C35/17
摘要： The present invention relates to a particularly economic overall method for producing menthol, specifically for producing optically active, essentially enantiomerically and diastereomerically pure L-menthol and racemic menthol, starting from the starting material citral which is available inexpensively on an industrial scale. The method has the following steps a.1) catalytic hydrogenation of neral and/or geranial to give citronellal, b.1) cyclization of citronellal to isopulegol in the presence of an acidic catalyst, c.1) purification of isopulegol by crystallization and d.1) catalytic hydrogenation of isopulegol to give menthol.
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![Method for the production of 4,4′-[1-(trifluoromethyl)alkylidene]-bis-(2,6-diphenylphenols)](/abs-image/US/2016/09/20/USRE46151E1/abs.jpg.150x150.jpg)
10.再颁专利Method for the production of 4,4′-[1-(trifluoromethyl)alkylidene]-bis-(2,6-diphenylphenols) 有权制备4,4' - [1-（三氟甲基）亚烷基] - 双（2,6-二苯基苯酚）公开(公告)号：USRE46151E1
公开(公告)日：2016-09-20
申请号：US14321865
申请日：2014-07-02
申请人： BASF SE
发明人： Gabriele Gralla , Gunnar Heydrich , Klaus Ebel , Wolfgang Krause
CPC分类号： C07C45/74 , C07C37/07 , C07C37/20 , C07C37/62 , C07C49/613 , C07C49/653 , C07C39/15 , C07C39/367
摘要： The present invention relates to a process for preparing 4,4′-[1-(trifluoromethyl)alkylidene]bis(2,6-diphenylphenols), in particular for preparing 4,4′-[1-(trifluoromethyl)ethylidene]bis(2,6-diphenylphenol), which comprises the self-condensation of cyclohexanone in the presence of a basic catalyst to form tricyclic condensation products, dehydrogenation of the resulting tricyclic condensation products in the presence of a supported transition metal catalyst in the condensed phase to form 2,6-diphenylphenol and reaction of the 2,6-diphenylphenol with a trifluoromethyl ketone. The invention further provides an improved process for preparing 2,6-diphenylphenol by aldol self-condensation of cyclohexanone.
摘要翻译： 本发明涉及一种制备4,4' - [1-（三氟甲基）亚烷基]双（2,6-二苯基苯酚）的方法，特别是制备4,4' - [1-（三氟甲基）亚乙基]双（ 2,6-二苯基苯酚），其包括环己酮在碱性催化剂存在下的自缩合以形成三环缩合产物，所得三环缩合产物在冷凝相中负载的过渡金属催化剂存在下脱氢形成 2,6-二苯基苯酚和2,6-二苯基苯酚与三氟甲基酮的反应。 本发明还提供了通过环己酮的醛醇自缩合制备2,6-二苯基苯酚的改进方法。
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