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    Process for the preparation of optically active 1H-furo[3,4-d]imidazole-2,4-diones
    11.
    发明专利
    Process for the preparation of optically active 1H-furo[3,4-d]imidazole-2,4-diones 未知

    公开(公告)号：DE3633887A1

    公开(公告)日：1988-04-07

    申请号：DE3633887

    申请日：1986-10-04

    Applicant: BASF AG

    Inventor： EGGERSDORFER MANFRED DR ,  SIEGEL HARDO DR

    IPC: C07D491/04 ,  C07D491/048 ,  C07D233/32

    Abstract: A process is proposed for the preparation of optically active 1H-furo[3,4-d]imidazole-2,4-diones of the general formula (I) in which R and R are identical or different and stand for hydrogen, C1-C3-alkyl, halogen or methoxy, which is characterised in that a mixture of diastereomeric imidazol-amide derivatives of the general formula (II) in which R and R have the meanings above, R is defined as R or R and R represents a group which is inert under liquid chromatographic conditions, but cannot denote hydrogen, is separated into the individual diastereomers using a solvent or solvent mixture on a column charged with a support material under liquid chromatographic conditions, and these diastereomers are then treated with acid.

    15.
    发明专利
    未知

    公开(公告)号：DE58901065D1

    公开(公告)日：1992-05-07

    申请号：DE58901065

    申请日：1989-03-22

    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.

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