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公开(公告)号：DE19853908A1
公开(公告)日：2000-06-08
申请号：DE19853908
申请日：1998-12-07
Applicant: BASF AG
Inventor： OOST CARSTEN , STROEZEL MANFRED , ETZRODT HEINZ , WELLER DIETMAR , KAIBEL GERD , JAEDICKE HAGEN
Abstract: Preparation of unsaturated methyl ketones(I), from an unsaturated alcohol(II) and alkyl acetoacetate(III) in the presence of an organo-aluminum catalyst(IV) comprises: (a) supplying (II) and (IV) to a reactor with a distillation column, (b) making temperature to be 170-250 degrees C under elevated pressure, (c) dosing the mixture with (III) and (d) maintaining a constant (III) content of 0.1-10 wt.% during the reaction. Preparation of unsaturated ketones of formula (I) involves reaction of an unsaturated alcohol of formula (II) with an alkyl acetoacetate of formula (III), in presence of 0.1-5 mol. % (based on (II)) of an organo-aluminum compound catalyst (IV), with elimination and distillative separation of the alcohol R3OH formed in the reaction, in a reactor system provided with a distillation column. Reaction is carried out by: (a) supplying (I (which boils at less than 140 degrees C), without a solvent, and (IV) to the reaction vessel, (b) adjusting the temperature to a value as constant as possible in the range 170-250 degrees C under elevated pressure, (c) dosing the mixture with (III) and (d) maintaining a (III) content as constant as possible in the range 0.1-10 wt. % during the reaction. Dotted line = optional bond; R1 = Me or Et; R2, R3 = 1-4C alkyl.
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公开(公告)号：DE19852691A1
公开(公告)日：2000-05-18
申请号：DE19852691
申请日：1998-11-16
Applicant: BASF AG
Inventor： OOST CARSTEN , STROEZEL MANFRED , ETZRODT HEINZ , WELLER DIETMAR , RHEUDE UDO , KAIBEL GERD , KRUG THOMAS , SPISKE LUISE , JAEDICKE HAGEN
IPC: B01J31/14 , C07B61/00 , C07C45/67 , C07C45/74 , C07C49/203
Abstract: Preparation of unsaturated ketones by reaction of the corresponding alpha , beta -unsaturated alcohol with an alkyl acetoacetate compound in the presence an organo-aluminum catalyst at constant temperature, with separation and continuous removal of CO2 and alcohol formed. Preparation of unsaturated ketones of formula (I) by reaction of the corresponding alpha , beta -unsaturated alcohol of formula (II) with an alkyl acetoacetate compound of formula (III) in the presence of 0.1-5 mole% (based on (III)) of an organo-aluminum catalyst with separation and continuous distillative removal of CO2 and alcohol of formula R3OH formed during reaction, in a reactor containing a fractionation column, where: (A) (II) is added to the reaction mixture together with the organic catalyst without additional solvent and (III) is then added to this mixture; (B) the reaction temperature is kept constant between 175-220 degrees C; (C) the content of (III) is kept at a constant level between 0.1-10 wt.% during the reaction. R1, R3 = 1-4C alkyl; R2 = 4-30C aliphatic, cycloaliphatic or cycloaliphatic-aliphatic; a, b = optional additional bonds.
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公开(公告)号：DE19815833A1
公开(公告)日：1999-10-14
申请号：DE19815833
申请日：1998-04-09
Applicant: BASF AG
Inventor： AQUILA WERNER , POX ROLAND , ETZRODT HEINZ
IPC: B01J31/04 , C07B61/00 , C07D311/72 , C07C67/46 , C07C69/14 , C07C69/145 , C07C69/157
Abstract: Alcohols or phenols are converted into acetate esters by reaction with an equimolar amount of keten in presence of a zinc carboxylate. Preparation of acetate esters (I) from organic compounds (II) containing one or more hydroxy groups is effected using an equimolar amount of keten based on the number of OH groups in (II), in presence of a zinc carboxylate salt (or zinc compound which forms zinc acetate under the reaction conditions), with intensive stirring of the reaction mixture.
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公开(公告)号：DE19815810A1
公开(公告)日：1999-10-14
申请号：DE19815810
申请日：1998-04-08
Applicant: BASF AG
Inventor： OOST CARSTEN , STROEZEL MANFRED , ETZRODT HEINZ , BOCKSTIEGEL BERNHARD , JAEDICKE HAGEN
Abstract: Preparation of psi , delta -unsaturated ketones (I) by modified Carroll reaction is catalysed by a stable liquid aluminum acetoacetate compound or mixture of such compounds. Some such catalyst mixtures are new. Preparation of psi , delta -unsaturated ketones of formula (I) involves modified Carroll reaction of an allyl alcohol of formula (II) with diketene or an alkyl acetoacetate of formula (III) in presence of an aluminum catalyst. R1 = H or 1-20C, saturated or unsaturated, branched hydrocarbyl; R2 = 1-5C alkyl. The novelty is that the catalyst consists of an aluminum compound (or aluminum compound mixture) which is a stable liquid at room temperature and contains at least one alkyl acetoacetate-forming group and 1 or 2 alkoxy groups or exclusively alkyl acetoacetate forming groups which are esterified sec. butanol or isobutanol or with at least two different alkanols. Independent claims are included for: (1) new mixtures of aluminum tris-acetoacetates of formula (V) which are liquid at room temperature; and (2) the preparation of mixtures as in (1). R3 = 1-5C alkyl, preferably Me or Et; R4 = 3-10C alkyl, preferably CHMe2, CH(Me)Et, CMe3 or CH(Me)-C3H7; R5 = 1-10C alkyl, preferably Me, Et, CHMe2, CH(Me)Et or CH(Me)-C3H7; provided that R3-R5 are not all the same. A further Independent claim relates to the continuous preparation of compounds (V) (or their mixtures), having the narrower proviso that R3-R5 can only be the same if they are -CH(Me)Et or -CH2CHMe2, which are liquid at room temperature. The process involves continuously reacting 1 mole of aluminum alcoholate of formula (VI) with 3-10 moles of (III), or with at least 3 moles of a mixture of 2 or 3 different compounds (III), optionally dissolved in an inert solvent. Reaction is at 100-250 (preferably 150-200) deg C and 1-100 (preferably 1-10) bars with a dwell time of 5-120 (preferably 15-45) minutes, the pressure and temperature being such that no gas phase is formed in the reaction vessel. R6 = 2-10C alkyl, preferably -CH2CHMe2, -CH(Me)Et or -CH(Me)C3H7; provided that R2 and R6 can only be the same if they are -CH(Me)Et or -CH2CHMe2.
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公开(公告)号：ES2175744T3
公开(公告)日：2002-11-16
申请号：ES98937471
申请日：1998-06-10
Applicant: BASF AG
Inventor： TELES JOAQUIM HENRIQUE , RIEBER NORBERT , BREUER KLAUS , DEMUTH DIRK , HIBST HARTMUT , ETZRODT HEINZ
Abstract: Enol ethers of the formula Iwhere 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 IIwith an acetylene or allene of the formula III or IVwhere 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.
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Patent Agency Ranking
公开(公告)号：DE59902731D1
公开(公告)日：2002-10-24
申请号：DE59902731
申请日：1999-11-13
Applicant: BASF AG
Inventor： OOST CARSTEN , STROEZEL MANFRED , ETZRODT HEINZ , WELLER DIETMAR , RHEUDE UDO , KAIBEL GERD , KRUG THOMAS , SPISKE LUISE , JAEDICKE HAGEN
IPC: B01J31/14 , C07B61/00 , C07C45/67 , C07C45/74 , C07C49/203
Abstract: Preparation of unsaturated ketones by reaction of the corresponding alpha , beta -unsaturated alcohol with an alkyl acetoacetate compound in the presence an organo-aluminum catalyst at constant temperature, with separation and continuous removal of CO2 and alcohol formed. Preparation of unsaturated ketones of formula (I) by reaction of the corresponding alpha , beta -unsaturated alcohol of formula (II) with an alkyl acetoacetate compound of formula (III) in the presence of 0.1-5 mole% (based on (III)) of an organo-aluminum catalyst with separation and continuous distillative removal of CO2 and alcohol of formula R3OH formed during reaction, in a reactor containing a fractionation column, where: (A) (II) is added to the reaction mixture together with the organic catalyst without additional solvent and (III) is then added to this mixture; (B) the reaction temperature is kept constant between 175-220 degrees C; (C) the content of (III) is kept at a constant level between 0.1-10 wt.% during the reaction. R1, R3 = 1-4C alkyl; R2 = 4-30C aliphatic, cycloaliphatic or cycloaliphatic-aliphatic; a, b = optional additional bonds.
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公开(公告)号：DE59803528D1
公开(公告)日：2002-05-02
申请号：DE59803528
申请日：1998-06-10
Applicant: BASF AG
Inventor： TELES HENRIQUE , RIEBER NORBERT , BREUER KLAUS , DEMUTH DIRK , HIBST HARTMUT , ETZRODT HEINZ , RHEUDE UDO
Abstract: Enol ethers of the formula Iwhere 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 IIwith an acetylene or allene of the formula III or IVwhere 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.
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公开(公告)号：DE19840747A1
公开(公告)日：2000-03-09
申请号：DE19840747
申请日：1998-09-07
Applicant: BASF AG
Inventor： OOST CARSTEN , STROEZEL MANFRED , ETZRODT HEINZ , WELLER DIETMAR , BOCKSTIEGEL BERNHARD , REIMER KLAUS , KAIBEL GERD , JAEDICKE HAGEN
IPC: B01J31/14 , B01D3/00 , B01D3/14 , B01D3/32 , B01J10/00 , B01J19/24 , C07B61/00 , C07C45/67 , C07C45/68 , C07C45/82 , C07C49/203 , C07C67/54 , C07C69/72 , C07C45/65 , C07C49/255
Abstract: Continuous production of 5-alken-2-one or 3,5-alkadien-2-one derivatives (I) by reacting a 1-alken-3-ol or 1-alkyn-3-ol derivative (II) with an alkyl acetoacetate (III) in a fractionation column to form an acetoacetate and alcohol involves (i) removing the alcohol and (ii) contacting the acetoacetate with catalyst in the lower part or bottom of the column to form (I). Continuous production of unsaturated ketones of formula (I) by reacting an unsaturated alcohol of formula (II) with an alkyl acetoacetate of formula (III) in the presence of an organoaluminum catalyst is carried out by: (a) reacting (II) with (III) on the plates of a fractionation column to form the acetoacetate of (II) and an alcohol of formula R OH; (b) removing the alcohol in the overhead stream from the column; (c) contacting the acetoacetate of (II) with the catalyst in the lower part or bottom of the column to form (I) and CO2; (d) removing the CO2 in the overhead stream from the column; and (e) withdrawing (I) in the bottoms stream from the column. R = 1-4C alkyl; R = 1-37C (un)saturated aliphatic hydrocarbyl (optionally substituted by methoxy groups), 4-12C cycloalkyl or 5-30C cycloalkylalkyl; and R = 1-5C alkyl.
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公开(公告)号：DE10123066A1
公开(公告)日：2002-11-14
申请号：DE10123066
申请日：2001-05-11
Applicant: BASF AG
Inventor： ANSMANN ANDREAS , HENKELMANN JOCHEM , KINDLER ALOIS , ETZRODT HEINZ , OOST CARSTEN , STUTZ SUSANNE , TRAGUT CHRISTIAN , BOCKSTIEGEL BERNHARD , REIMER KLAUS , STROEZEL MANFRED , DOBLER WALTER
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公开(公告)号：DE19936208A1
公开(公告)日：2001-02-15
申请号：DE19936208
申请日：1999-08-02
Applicant: BASF AG
Inventor： BROECKER FRANZ JOSEF , AQUILA WERNER , BUECHELE WOLFGANG , ETZRODT HEINZ , SCHAEFER-LUEDERSSEN ULRICH , SCHWAB EKKEHARD
Abstract: A continuous process for the production of 2-phenylethanol from styrene oxide by hydrogenation of a solution containing styrene oxide and 2-phenylethanol with hydrogen in the presence of a catalyst comprising a monolithic supported catalyst having a metallic support. An Independent claim is included for a device for carrying out the process, comprising a reactor (1) containing the catalyst (2) having an inlet at the base of the reactor by which the reaction solution and hydrogen enters the reactor via liquid-spray gas compressor (5). The reaction mixture leaves the reactor by the outlet (6) to a separator (7) from which the product is recovered (14) and the reaction solution containing the unreacted material is recirculated by means of the pump (8), heat exchanger (9) and liquid-spray gas compressor (5). Fresh reactant is introduced by means of (3). Unreacted hydrogen from the separator (7) is recirculated via a gas recirculation loop comprising pipes (11) and (13) and liquid-spray gas compressor (5). Fresh hydrogen is added by means of (4) and pressure is maintained by means of the gas outlet (12).
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