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    • 23. 发明专利
    • DE59306312D1
    • 1997-06-05
    • DE59306312
    • 1993-07-08
    • BASF AG
    • KRAUSE WOLFGANG DRPAUST JOACHIM DRDOBLER WALTER DRJAEDICKE HAGEN DR
    • C07F9/54C07D319/06C07F9/655
    • 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.
    • 29. 发明专利
    • DE3905765A1
    • 1990-08-30
    • DE3905765
    • 1989-02-24
    • BASF AG
    • HUEMMER WOLFGANG DRDOBLER WALTER DRLITTMANN DIETER DR
    • G03F7/004G03F7/027G03F7/031G03F7/032
    • 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.
    • 30. 发明专利
    • DE3810957A1
    • 1989-10-19
    • DE3810957
    • 1988-03-31
    • BASF AG
    • DOBLER WALTER DREGGERSDORFER MANFRED DRPAUST JOACHIM DR
    • C07D475/14C07F9/547C07F9/6561
    • 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.