公开(公告)号：JPH10265419A

公开(公告)日：1998-10-06

申请号：JP4200698

申请日：1998-02-24

Applicant: BASF AG

Inventor： KIEFER MATTHIAS DR ,  SIEGEL WOLFGANG DR ,  THERRE JOERG DR ,  PAHL MELANIE ,  AQUILA WERNER DR ,  SCHAEFER-LUEDERSSEN ULRICH DR ,  RHEUDE UDO DR

IPC: C07B61/00 ,  C07C29/56 ,  C07C33/02 ,  C07C33/03

Abstract: PROBLEM TO BE SOLVED: To provide a method for isomerizing ally alcohol in high yield and selectivity, and at a low cost. SOLUTION: In a method in which allyl alcohol of a starting material is isomerized to allyl alcohol of a product in an aqueous solution in the presence of a protonic acid, the pH value of the reaction mixture is adjusted in the range of 2-5 with a protonic acid at a concentration of

公开(公告)号：JP2000119211A

公开(公告)日：2000-04-25

申请号：JP28441399

申请日：1999-10-05

Applicant: BASF AG

Inventor： THERRE JOERG DR ,  KAIBEL GERD DR ,  AQUILA WERNER DR ,  WEGNER GUENTER ,  FUCHS HARTWIG

IPC: B01J27/16 ,  C07B61/00 ,  C07C41/28 ,  C07C43/15 ,  C07C45/37 ,  C07C45/51 ,  C07C45/54 ,  C07C45/67 ,  C07C47/21 ,  C07C49/203

Abstract: PROBLEM TO BE SOLVED: To provide a method for producing citral in a high yield by continuously distilling out formed intermediate compounds, such as prenol, as well as the citral from a reaction mixture during reactions, and heating the intermediate compounds at a specified temperature, when a specific acetal is thermally decomposed to form the prenol and the dienyl ether, and then the formed ether is subjected to Claisen rearrangement and subsequently to Cope rearrangement. SOLUTION: This method for producing citral of formula V comprises thermally decomposing (A) 3-methyl-2-buten-1-al-diprenyl acetal of formula I, if necessary, in the presence of an acidic catalyst, to form (B) prenol of formula II and (C) a compound of formula III, subjecting the formed compound of formed III to Claisen rearrangement to obtain (D) formylhexadiene of formula IV, and subsequently subjecting the obtained compound to Cope rearrangement. Therein, the characteristics comprise continuously distilling out the formed intermediate compounds of the component B, the component C and the component D as well as the objective citral from the reaction mixture during the above reactions, and heating the prenol and, if necessary, the intermediate compounds of the component C and D at 100-200 deg.C.

公开(公告)号：JPH11292809A

公开(公告)日：1999-10-26

申请号：JP6554099

申请日：1999-03-11

Applicant: BASF AG

Inventor： KIEFER MATTHIAS DR ,  SIEGEL WOLFGANG DR ,  THERRE JOERG DR ,  PAHL MELANIE ,  AQUILA WERNER DR ,  SCHAEFER-LUEDERSSEN ULRICH DR

IPC: C07C29/56 ,  C07C29/80 ,  C07C33/02 ,  C07C33/03

Abstract: PROBLEM TO BE SOLVED: To provide a simple, inexpensive and extremely selective method for continuously producing pure dimethylvinylcarbinol(DMVC) from prenol provided with a high space time yield. SOLUTION: (a) The formation of a liquid two-phase mixture in a reactional mixture is avoided during a reaction as far as possible, (b) a formed DMVC is distilled in a reflux ratio of at least 2 and (c) the reactional volume and/or the amount of the prenol added per h and/or the concentration of a protonic acid in the reactional mixture are set so as to provide the product of the quotient obtained by dividing the reactional volume divided by the prenol volume added per h and the proton concentration in the reactional mixture defined as a residence time concentration coefficient with a value of 0.001 h.mol/L to 1 h.mol/L in a method for continuously reacting the prenol with an aqueous solution of the protonic acid in a still or a rectifying column while distilling off the DMVC formed in the state of an azeotropic mixture with water and thereby producing the DMVC.

公开(公告)号：DE19738083A1

公开(公告)日：1999-03-04

申请号：DE19738083

申请日：1997-09-01

Applicant: BASF AG

Inventor： KIEFER MATTHIAS DR ,  SIEGEL WOLFGANG DR ,  THERRE JOERG DR ,  PAHL MELANIE

IPC: C07C29/56 ,  C07C33/03

Abstract: In the isomerisation of educt allyl alcohols (I) to product allyl alcohols (II) in aqueous solution in the presence of protonic acid (III), the pH of the reaction mixture is adjusted to 2-5 with (III) in a concentration 0.16 mole/l reaction mixture or a buffer containing (III).

公开(公告)号：DE59402009D1

公开(公告)日：1997-04-17

申请号：DE59402009

申请日：1994-06-15

Applicant: BASF AG

Inventor： THERRE JOERG DR ,  SCHWARZ HANS VOLKMAR DR ,  AGAR DAVID DR

IPC: C07C67/14 ,  C07C67/60 ,  C07C69/80

公开(公告)号：DE4322548A1

公开(公告)日：1995-01-12

申请号：DE4322548

申请日：1993-07-07

Applicant: BASF AG

Inventor： THERRE JOERG DR ,  SCHWARZ HANS VOLKMAR DR

IPC: C07C263/00 ,  C07C263/20 ,  C07C265/14

Abstract: The invention relates to a process for the disposal of solid residues of toluylene diisocyanate preparation by treatment of the solid residues which preferably have an NCO content of at most 1% by weight, at elevated temperatures, expediently at temperatures from 85 to 300 DEG C, and optionally elevated pressure, with at least one reactive compound from the group consisting of mono- and polyhydric alcohols, mono- and polycarboxylic acids, hydroxycarboxylic acids, carboxylic acid or hydroxycarboxylic acid esters and lactones or mixtures thereof for liquefaction thereof and subsequent incineration thereof in liquid form.

公开(公告)号：SI0941979T1

公开(公告)日：2002-10-31

申请号：SI9930069

申请日：1999-03-05

Applicant: BASF AG

Inventor： KIEFER MATTHIAS DR ,  SIEGEL WOLFGANG DR ,  THERRE JOERG DR ,  PAHL MELANIE ,  AQUILA WERNER DR ,  SCHAEFER-LUEDERSSEN ULRICH DR

IPC: C07C29/56 ,  C07C29/80 ,  C07C33/02 ,  C07C33/03

Abstract: Continuous production of dimethyl vinyl carbinol (DMVC) comprises reaction of prenol with an aqueous solution of a protonic acid in the bottom or upper part of a rectification column while distilling off the DMVC as an azeotropic mixture with water under specified conditions. Continuous production of dimethyl vinyl carbinol (DMVC) by reaction of prenol with an aqueous solution of a protonic acid in the bottom or upper part of a rectification column while distilling off the DMVC as an azeotropic mixture with water is performed in such a way that (a) the amount of liquid two-phase mixture formed during the reaction is minimized, (b) the DMVC is distilled off with a reflux ratio of at least 2, and (c) the reaction volume (V in ml) and/or the amount of prenol added per hour (P in ml/hour) and/or the proton concentration in the reaction mixture (C in moles/liter) is such that VC/P = 0.001-1 h.mol/l.

公开(公告)号：DE59901582D1

公开(公告)日：2002-07-11

申请号：DE59901582

申请日：1999-03-05

Applicant: BASF AG

Inventor： KIEFER MATTHIAS DR ,  SIEGEL WOLFGANG DR ,  THERRE JOERG DR ,  PAHL MELANIE ,  AQUILA WERNER DR ,  SCHAEFER-LUEDERSSEN ULRICH DR

IPC: C07C29/56 ,  C07C29/80 ,  C07C33/02 ,  C07C33/03

Abstract: Continuous production of dimethyl vinyl carbinol (DMVC) comprises reaction of prenol with an aqueous solution of a protonic acid in the bottom or upper part of a rectification column while distilling off the DMVC as an azeotropic mixture with water under specified conditions. Continuous production of dimethyl vinyl carbinol (DMVC) by reaction of prenol with an aqueous solution of a protonic acid in the bottom or upper part of a rectification column while distilling off the DMVC as an azeotropic mixture with water is performed in such a way that (a) the amount of liquid two-phase mixture formed during the reaction is minimized, (b) the DMVC is distilled off with a reflux ratio of at least 2, and (c) the reaction volume (V in ml) and/or the amount of prenol added per hour (P in ml/hour) and/or the proton concentration in the reaction mixture (C in moles/liter) is such that VC/P = 0.001-1 h.mol/l.

公开(公告)号：SI0992477T1

公开(公告)日：2003-06-30

申请号：SI9930238

申请日：1999-09-17

Applicant: BASF AG

Inventor： THERRE JOERG DR ,  KAIBEL GERD DR ,  AQUILA WERNER DR ,  WEGNER GUENTER DR ,  FUCHS HARTWIG

IPC: C07B61/00 ,  C07C41/28 ,  B01J27/16 ,  C07C43/15 ,  C07C45/37 ,  C07C45/51 ,  C07C45/54 ,  C07C45/67 ,  C07C47/21 ,  C07C49/203

Abstract: Preparation of citral (I) comprises thermal decomposition of 3-methyl-2-buten-1-al-diprenylacetal and rearrangement of obtained intermediates cis/trans-prenyl-(methyl-butadienyl)-ether (IV) and 2,4,4-trimethyl-3-formyl-1,5-hexadiene (V). (IV) and (V) are continuously distilled off and converted into (I) before or after removal of by-product prenol. Preparation of 3,7-dimethyl-2,6-octadien-1-al (citral) of formula (I) comprises: (1) thermal decomposition of 3-methyl-2-buten-1-al-diprenylacetal of formula (II) optionally in the presence of an acid catalyst to split off 3-methyl-buten-1-ol (prenol) of formula (III) and form cis/trans-prenyl-(methyl-butadienyl)-ether of formula (IV); (2) Claisen rearrangement of (IV) to give 2,4,4-trimethyl-3-formyl-1,5-hexadiene of formula (V); and (3) Cope rearrangement of (V) to form (I). The transitionally formed (IV) and (V) and the desired citral as well as the prenol (III) are continuously distilled out of the reaction mixture and (IV) and (V), before or after distillative separation of (III) and optional by-products, are subjected to rearrangement to form (I) at 100-200 degrees C.

公开(公告)号：DK0992477T3

公开(公告)日：2003-02-24

申请号：DK99118458

申请日：1999-09-17

Applicant: BASF AG

Inventor： THERRE JOERG DR ,  KAIBEL GERD DR ,  AQUILA WERNER DR ,  WEGNER GUENTER DR ,  FUCHS HARTWIG

IPC: B01J27/16 ,  C07B61/00 ,  C07C41/28 ,  C07C43/15 ,  C07C45/37 ,  C07C45/51 ,  C07C45/54 ,  C07C45/67 ,  C07C47/21 ,  C07C49/203

Abstract: Preparation of citral (I) comprises thermal decomposition of 3-methyl-2-buten-1-al-diprenylacetal and rearrangement of obtained intermediates cis/trans-prenyl-(methyl-butadienyl)-ether (IV) and 2,4,4-trimethyl-3-formyl-1,5-hexadiene (V). (IV) and (V) are continuously distilled off and converted into (I) before or after removal of by-product prenol. Preparation of 3,7-dimethyl-2,6-octadien-1-al (citral) of formula (I) comprises: (1) thermal decomposition of 3-methyl-2-buten-1-al-diprenylacetal of formula (II) optionally in the presence of an acid catalyst to split off 3-methyl-buten-1-ol (prenol) of formula (III) and form cis/trans-prenyl-(methyl-butadienyl)-ether of formula (IV); (2) Claisen rearrangement of (IV) to give 2,4,4-trimethyl-3-formyl-1,5-hexadiene of formula (V); and (3) Cope rearrangement of (V) to form (I). The transitionally formed (IV) and (V) and the desired citral as well as the prenol (III) are continuously distilled out of the reaction mixture and (IV) and (V), before or after distillative separation of (III) and optional by-products, are subjected to rearrangement to form (I) at 100-200 degrees C.