公开(公告)号：DE59904211D1

公开(公告)日：2003-03-13

申请号：DE59904211

申请日：1999-10-05

Applicant: BASF AG

Inventor： RUFF DR ,  BAUMANN DIETER ,  AQUILA DR ,  SCHUBERT DR ,  LECHTKEN DR

IPC: B01J31/22 ,  C07B61/00 ,  C07C46/08 ,  C07C46/10 ,  C07C50/02 ,  C07C50/04

Abstract: Purification of 2,3,5-trimethyl-p-benzoquinone (TMQ) or isolation of TMQ from a mixture, by crystallization. An Independent claim is included for preparation of TMQ by catalytic oxidation of TMP with oxygen to give a mixture containing TMQ as well as TMP and/or at least 1 of solvent, catalyst-residue, by-product and intermediate, followed by work-up as above.

公开(公告)号：DE59802205D1

公开(公告)日：2002-01-10

申请号：DE59802205

申请日：1998-05-13

Applicant: BASF AG

Inventor： AQUILA DR ,  FUCHS HARTWIG ,  WOERZ DR ,  RUPPEL DR ,  HALBRITTER DR

IPC: B01J23/52 ,  B01J8/02 ,  B01J8/08 ,  C07B61/00 ,  C07C45/38 ,  C07C45/67 ,  C07C47/21 ,  C07C47/22

Abstract: Continuous technical preparation of aldehydes of formula (I) comprises dehydration of the corresponding alcohol of formula (II) with an oxygen-containing gas using a catalyst based on copper, silver and/or gold on an inert carrier in a multi-pipe reactor. This is followed by rapid cooling of the reaction gases, separation of the aldehyde from the resulting condensate and recycling of any unreacted alcohol. During the process (II) is vapourised, the alcohol vapour is mixed with the oxygen-containing gas, the resulting vapour is passed through a 0.5 cm layer of the catalyst at a temperature that is greater than the boiling point of the alcohol but lower than the starting temperature of the reaction and the vapour is then allowed to pass through a number of parallel pipes which are filled with catalyst and kept warm by a circulating fluid. The pipes have an inner diameter, D, of 0.5-3 cm and are at least 5 cm long and the reaction temperature is 300-600 degrees C. R1R2CHO (I) R1R2CH-CH2-OH (II) R1 = H and R2 = CH2=C(CH3)- (isoprenal); or R1+R2 = (CH3)2C= (prenal)

公开(公告)号：DE50100896D1

公开(公告)日：2003-12-11

申请号：DE50100896

申请日：2001-08-25

Applicant: BASF AG

Inventor： THERRE DR ,  KAIBEL DR ,  AQUILA DR ,  WEGNER DR ,  FUCHS HARTWIG

IPC: C07C41/50 ,  C07B61/00 ,  C07C41/56 ,  C07C41/58 ,  C07C43/303

Abstract: Preparation of acetals by reaction of 1 mol. of an unsaturated aldehyde with 1 mol. of an unsaturated alcohol in presence of an acid as catalyst and with separation of the water of reaction is effected by partly reacting the reactants in a column, concentrating the obtained acetal in ≥ 2 sequential evaporation steps and then recycling the recovered reactants to the reaction column. Preparation of acetals (I) by reaction of 1 mol. of an unsaturated aldehyde (II) with 1 mol. of an unsaturated alcohol (III) in presence of an acid as catalyst and with separation of the water of reaction is effected by partly reacting the reactants in a column, concentrating the obtained acetal in ≥ 2 sequential evaporation steps and then recycling the recovered reactants to the reaction column. R - R = H or optionally substituted 1-6C alkyl; and R = H, an optionally mono- or poly-unsaturated, optionally substituted 1-12C alkyl or an optionally substituted 3-12-membered optionally mono- or poly-unsaturated carbon ring.

公开(公告)号：DE59904210D1

公开(公告)日：2003-03-13

申请号：DE59904210

申请日：1999-09-17

Applicant: BASF AG

Inventor： THERRE DR ,  KAIBEL DR ,  AQUILA DR ,  WEGNER 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.

公开(公告)号：DE59903948D1

公开(公告)日：2003-02-13

申请号：DE59903948

申请日：1999-03-25

Applicant: BASF AG

Inventor： AQUILA DR ,  POX ROLAND ,  ETZRODT DR

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.

公开(公告)号：DE59806481D1

公开(公告)日：2003-01-16

申请号：DE59806481

申请日：1998-02-20

Applicant: BASF AG

Inventor： KIEFER DR ,  SIEGEL DR ,  THERRE DR ,  PAHL MELANIE ,  AQUILA DR ,  SCHAEFER-LUEDERSSEN DR ,  RHEUDE DR

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

公开(公告)号：DE59903222D1

公开(公告)日：2002-12-05

申请号：DE59903222

申请日：1999-03-26

Applicant: BASF AG

Inventor： BROECKER DR ,  KAIBEL DR ,  AQUILA DR ,  FUCHS HARTWIG ,  WEGNER DR ,  STROEZEL MANFRED

IPC: B01J23/44 ,  B01J8/20 ,  B01J8/22 ,  B01J19/24 ,  B01J23/46 ,  C07B61/00 ,  C07C45/62 ,  C07C47/21 ,  C07C49/04

Abstract: Production of saturated carbonyl compounds (I) by selective liquid-phase hydrogenation of alpha , beta -unsaturated carbonyl compounds (II) is carried out in a packed bubble column with the product recycled and by circulating hydrogen gas. Production of saturated carbonyl compounds of formula R1-CH(R2)-CH(R3)-C(R4)=O (I) by selective liquid-phase hydrogenation of alpha , beta -unsaturated carbonyl compounds of formula R1-C(R2)=C(R3)-C(R4)=O (II) in the presence of a particulate palladium and/or rhodium catalyst and a base is carried out in a packed bubble column with the product recycled and by circulating hydrogen gas. R1 = H or an organic group; R2-R4 = H or 1-4C alkyl.