公开(公告)号：DE59308496D1

公开(公告)日：1998-06-10

申请号：DE59308496

申请日：1993-08-27

Applicant: BASF AG

Inventor： PAUST JOACHIM DR ,  ECKES PETER DR ,  SIEGEL WOLFGANG DR ,  BALKENHOHL FRIEDHELM DR ,  DOBLER WALTER DR ,  HUELLMANN MICHAEL DR

IPC: C07C323/52 ,  C07C67/00 ,  C07C69/06 ,  C07C69/708 ,  C07C319/08 ,  C07D339/04

公开(公告)号：DE59500893D1

公开(公告)日：1997-12-04

申请号：DE59500893

申请日：1995-06-30

Applicant: BASF AG

Inventor： DOBLER WALTER DR ,  KRAUSE WOLFGANG DR ,  PAUST JOACHIM DR ,  WOERZ OTTO DR ,  RHEUDE UDO DR ,  BURST WOLFRAM ,  DAEUWEL GUENTER ,  BERTRAM ARMIN ,  SCHULZ BERNHARD DR ,  WEGNER GUENTER DR ,  MUENSTER PETER DR ,  ERNST HANSGEORG DR ,  KOCHNER ARNO ,  ETZRODT HEINZ DR

IPC: C07C51/16 ,  C07C403/00 ,  C07C403/20

公开(公告)号：DE59306312D1

公开(公告)日：1997-06-05

申请号：DE59306312

申请日：1993-07-08

Applicant: BASF AG

Inventor： KRAUSE WOLFGANG DR ,  PAUST JOACHIM DR ,  DOBLER WALTER DR ,  JAEDICKE HAGEN DR

IPC: C07F9/54 ,  C07D319/06 ,  C07F9/655

Abstract: Improved process for preparing cyclic acetals of 3-formyl-2-butenyltriphenylphosphonium chloride by acetalisation of 3-formyl-2-butenyl acetate with an aliphatic 1,3-diol, conversion of the 4-acetoxyacetal obtained into the corresponding 4-hydroxyacetal, Vilmeier chlorination to give the corresponding 4-chloroacetal and subsequent reaction with triphenylphosphine, which is characterised in that the first 3 reaction steps are carried out in an aliphatic or cycloaliphatic hydrocarbon or hydrocarbon mixture having 6 to 8 C atoms and the reaction with triphenylphosphine is carried out in an alkanol having 1 to 3 C atoms and/or in an aliphatic or cycloaliphatic hydrocarbon having 6 to 8 C atoms or an appropriate hydrocarbon mixture. The process becomes particularly advantageous if the conversion of the 4-acetoxyacetal into the 4-hydroxyacetal is carried out with an aqueous alkali solution and in the presence of phase-transfer catalysts and the first three or all four reaction steps are carried out in the same C6-to C8-hydrocarbon.

公开(公告)号：DE59009603D1

公开(公告)日：1995-10-12

申请号：DE59009603

申请日：1990-03-20

Applicant: BASF AG

Inventor： DOBLER WALTER DR ,  PAUST JOACHIM DR ,  BETZ ROLAND DR

IPC: C07F9/09 ,  C07F9/655

公开(公告)号：ES2051962T3

公开(公告)日：1994-07-01

申请号：ES89120519

申请日：1989-11-06

Applicant: BASF AG

Inventor： HERMELING DIETER DR ,  BECKER RAINER DR ,  DOBLER WALTER DR

IPC: C07C49/17 ,  C25B3/29 ,  C25B3/10

Abstract: Method for the preparation of dihydroxydiones of the general formula R-CO-CH(OH)-CH(OH)-CO-R I in which R stands for an alkyl radical, in which an aldehyde of the general formula in which R has the abovementioned meaning, is electrolysed in a water- containing electrolyte which has a pH of less than 7.

公开(公告)号：DE4225322A1

公开(公告)日：1994-02-03

申请号：DE4225322

申请日：1992-07-31

Applicant: BASF AG

Inventor： KRAUSE WOLFGANG DR ,  PAUST JOACHIM DR ,  DOBLER WALTER DR ,  JAEDICKE HAGEN DR

IPC: C07D319/06 ,  C07F9/655 ,  B01J27/20

Abstract: Prodn. of 3-formyl-2-butenyl-triphenylphosphonium chloride cyclic acetals of formula (I) is effected by: (a) reacting 3-formyl-2-butenyl acetate (II) with a 1,3-diol of formula (III) in a 6-8C aliphatic or alicyclic hydrocarbon solvent (S1); (b) converting the resulting acetoxy acetal of formula (IV) to the corresp. hydroxy acetal of formula (V) in S1; (c) subjecting (V) to Vilsmeier chlorination in S1; and (d) reacting the resulting choro acetal of formula (VI) with PPh3 in a 1-3C alkanol and/or S1. In the formula, R1-R4 = H or Me. Also claimed is a process for preparing (I) comprising step (d) as above. Step (b) is effected by reaction with at least 5% aq. NaOH or KOH in the presence of a phase transfer catalyst. Step (d) is effected in a mixt. of MeOH and S1.

公开(公告)号：DE4223061A1

公开(公告)日：1994-01-20

申请号：DE4223061

申请日：1992-07-14

Applicant: BASF AG

Inventor： KRAUSE WOLFGANG DR ,  PAUST JOACHIM DR ,  DOBLER WALTER DR ,  JAEDICKE HAGEN DR

IPC: C07D319/06 ,  C07F9/655

Abstract: Prodn. of 3-formyl-2-butenyl-triphenylphosphonium chloride cyclic acetals of formula (I) is effected by: (a) reacting 3-formyl-2-butenyl acetate (II) with a 1,3-diol of formula (III) in a 6-8C aliphatic or alicyclic hydrocarbon solvent (S1); (b) converting the resulting acetoxy acetal of formula (IV) to the corresp. hydroxy acetal of formula (V) in S1; (c) subjecting (V) to Vilsmeier chlorination in S1; and (d) reacting the resulting choro acetal of formula (VI) with PPh3 in a 1-3C alkanol and/or S1. In the formula, R1-R4 = H or Me. Also claimed is a process for preparing (I) comprising step (d) as above. Step (b) is effected by reaction with at least 5% aq. NaOH or KOH in the presence of a phase transfer catalyst. Step (d) is effected in a mixt. of MeOH and S1.

公开(公告)号：DE4000977A1

公开(公告)日：1991-07-18

申请号：DE4000977

申请日：1990-01-16

Applicant: BASF AG

Inventor： DOBLER WALTER DR ,  BALKENHOHL FRIEDHELM DR ,  BETZ ROLAND DR ,  PAUST JOACHIM DR

IPC: C07F9/655

Abstract: K-Mg L-ascorbate-2-phosphate (I) is a new cpd. Pref., it has K:Mg atom ratio 1 +/- 0.3 : 1 +/- 0.15. The salt is prepd. by treating aq. soln. of K L-ascorbate-2-phosphate (III) with a medium-acidity cation exchanger which loses its exchange capacity at pH 2-0.5 to produce a soln. of mono-K salt. This is treated with MgO, Mg(OH)2 or MgCO3 to about pH7 and the soln. opt. treated with MeOH or acetone to ppte. (I). USE/ADVANTAGE - Conversion to (I) is used to recover L-ascorbic acid-2-phosphate (II) from phosphorylation mixt. It is produced free of inorganic salts; in well-crystallisation form which is easy to filter, non-hygroscopic and has little tendency to cake or form dust. The use of a medium-acidity resin produces an eluate which is not strongly acid (so does not decompose the product); MgO consumption and salt discharge are reduced, and regeneration times for the resin are Compared with ascorbic acid itself, (II) is more stable to oxygen, heat and hydrolysis, and has universal bioavailability.

公开(公告)号：DE3905765A1

公开(公告)日：1990-08-30

申请号：DE3905765

申请日：1989-02-24

Applicant: BASF AG

Inventor： HUEMMER WOLFGANG DR ,  DOBLER WALTER DR ,  LITTMANN DIETER DR

IPC: G03F7/004 ,  G03F7/027 ,  G03F7/031 ,  G03F7/032

Abstract: Photosensitive recording element containing at least one photopolymerisable recording layer (B) composed of… b1) at least one partially or virtually completely hydrolysed poly(vinylalcohol alkane carboxylate) and/or at least one partially or virtually completely hydrolysed vinyl alcohol alkane carboxylate/alkylene oxide graft copolymer as binder,… b2) at least one photopolymerisation initiator,… b3) at least one photopolymerisable olefinically unsaturated compound (monomer) which is compatible with the binder (b1), and/or photopolymerizable olefinically unsaturated radicals which are linked laterally and/or terminally to the binder (b1), and… b4) at least two auxiliaries, the photopolymerizable recording layer (B) containing, as auxiliaries (b4), at least the sensitometric regulator (b4) composed of… b4.1) at least one compound from the class comprising the isoalloxazines and/or the class comprising the alloxazines, and also… b4.2) the potassium salt of N-nitrosocyclohexyl hydroxylamine, N-nitrosodiphenylamine and/or the monomethyl ether of hydroquinone in an amount of 0,01 to 6% by weight of the photopolymerizable recording layer (B), the (b4.1):(b4.2) weight ratio being 1:2 to 1:1000.

公开(公告)号：DE3810957A1

公开(公告)日：1989-10-19

申请号：DE3810957

申请日：1988-03-31

Applicant: BASF AG

Inventor： DOBLER WALTER DR ,  EGGERSDORFER MANFRED DR ,  PAUST JOACHIM DR

IPC: C07D475/14 ,  C07F9/547 ,  C07F9/6561

Abstract: Process for the purification of salts of riboflavin 5'-phosphate obtained by phosphorylation of riboflavin and reaction of the riboflavin 5'-phosphate (5'-FMN) contaminated with unreacted riboflavin and isomeric riboflavin monophosphates and diphosphates and formed in this process with alkali metal hydroxides or nitrogen bases, which is characterised in that a) an approximately 1 to 15% strength by weight homogeneous, clear, aqueous 5'-FMN salt solution having a pH from 4 to 7 is prepared from the crude 5'-FMN obtained in the phosphorylation, water, and the alkali metal hydroxide or the nitrogen base, preferably sodium hydroxide solution, optionally with warming at 30 to 100 DEG C, b) the solution obtained is treated with a suitable polymeric adsorber resin and c) the 5'-FMN salt largely purified of unreacted riboflavin is isolated from the solution obtained in this process and, if desired, the solution is submitted to a subsequent fine purification. The treatment with the suitable polymeric adsorber resin is advantageously carried out in a column packed with adsorber resin. The subsequent fine purification can be carried out by means of crystallisation by evaporation or by chromatography of a 5'-FMN solution containing 1 to 15% by weight of dry material in water or a mixture of water and a lower aliphatic alcohol having a pH between 4 and 7 in a minimum amount of 5 to 50% of the bed volume of the column on RP silica gel derivatised with alkyl groups using water or a mixture of water and a lower aliphatic alcohol as the eluent. The preparative chromatography of 5'-FMN salts on derivatised RP silica gel with water or a mixture of water and a lower aliphatic alcohol as the solvent and eluent is also claimed independently of the pretreatment with the suitable adsorber resin.