32.
    发明专利
    未知

    公开(公告)号:DK163060C

    公开(公告)日:1992-06-09

    申请号:DK260285

    申请日:1985-06-11

    Applicant: BASF AG

    Abstract: Very pure riboflavin (I) is obtained by a process in which the riboflavin is dissolved in dilute aqueous alkali metal hydroxide solution, if necessary the alkaline solution is purified by treatment with active carbon or with a solvent which is insoluble or only slightly soluble in water, the resulting alkaline solution of I is introduced into water which is at 90 DEG -100 DEG C. and to which an acid has been added in an amount such that the reaction mixture is brought to a pH of from 6.5 to 0.8, the temperature being maintained at from 40 DEG to 100 DEG C., the reaction mixture is kept at from 90 DEG to 100 DEG C. for from 10 to 80 minutes and cooled, and I is then isolated.

    33.
    发明专利
    未知

    公开(公告)号:DK162229C

    公开(公告)日:1992-03-16

    申请号:DK589383

    申请日:1983-12-21

    Applicant: BASF AG

    Abstract: An improved process for the purification of crude riboflavin which has been prepared by condensation of an N-(D)-ribityl-2-arylazo-4,5-dimethylaniline and barbituric acid or another N-(D)-ribityl-4,5-dimethyl-aniline derivative with a barbituric acid derivative, by dissolving the crude riboflavin in sulfuric acid or phosphoric acid which has been diluted with water and oxidizing the impurities by treating the solution with hydrogen peroxide, or by dissolving the riboflavin in dilute nitric acid at elevated temperature and then isolating the pure riboflavin by precipitation with water, wherein the mineral acid solution of the riboflavin and the oxidizing agent or the solution of the riboflavin in 20 to 70% strength by weight nitric acid is heated extremely rapidly to a temperature at which the solution clearly changes color from greenish to yellow-orange, the solution is kept at this temperature for from 1 to 50, seconds and the oxidation reaction is then interrupted by addition of water. The best results are achieved in this process if from 20 to 65% strength by weight nitric acid is used simultaneously as the acid and oxidative agent and if, after the change in color, the mineral acid solution, in particular the nitric acid solution, is passed, immediately or after prior interruption of the oxidation reaction by addition of cold water, into hot water at from 90 DEG to 100 DEG C. and the suspension thereby formed is kept at this temperature for about a further 10-30 minutes.

    34.
    发明专利
    未知

    公开(公告)号:DK162229B

    公开(公告)日:1991-09-30

    申请号:DK589383

    申请日:1983-12-21

    Applicant: BASF AG

    Abstract: An improved process for the purification of crude riboflavin which has been prepared by condensation of an N-(D)-ribityl-2-arylazo-4,5-dimethylaniline and barbituric acid or another N-(D)-ribityl-4,5-dimethyl-aniline derivative with a barbituric acid derivative, by dissolving the crude riboflavin in sulfuric acid or phosphoric acid which has been diluted with water and oxidizing the impurities by treating the solution with hydrogen peroxide, or by dissolving the riboflavin in dilute nitric acid at elevated temperature and then isolating the pure riboflavin by precipitation with water, wherein the mineral acid solution of the riboflavin and the oxidizing agent or the solution of the riboflavin in 20 to 70% strength by weight nitric acid is heated extremely rapidly to a temperature at which the solution clearly changes color from greenish to yellow-orange, the solution is kept at this temperature for from 1 to 50, seconds and the oxidation reaction is then interrupted by addition of water. The best results are achieved in this process if from 20 to 65% strength by weight nitric acid is used simultaneously as the acid and oxidative agent and if, after the change in color, the mineral acid solution, in particular the nitric acid solution, is passed, immediately or after prior interruption of the oxidation reaction by addition of cold water, into hot water at from 90 DEG to 100 DEG C. and the suspension thereby formed is kept at this temperature for about a further 10-30 minutes.

    35.
    发明专利
    未知

    公开(公告)号:DK260285D0

    公开(公告)日:1985-06-11

    申请号:DK260285

    申请日:1985-06-11

    Applicant: BASF AG

    Abstract: Very pure riboflavin (I) is obtained by a process in which the riboflavin is dissolved in dilute aqueous alkali metal hydroxide solution, if necessary the alkaline solution is purified by treatment with active carbon or with a solvent which is insoluble or only slightly soluble in water, the resulting alkaline solution of I is introduced into water which is at 90 DEG -100 DEG C. and to which an acid has been added in an amount such that the reaction mixture is brought to a pH of from 6.5 to 0.8, the temperature being maintained at from 40 DEG to 100 DEG C., the reaction mixture is kept at from 90 DEG to 100 DEG C. for from 10 to 80 minutes and cooled, and I is then isolated.

    36.
    发明专利
    未知

    公开(公告)号:DK79685D0

    公开(公告)日:1985-02-21

    申请号:DK79685

    申请日:1985-02-21

    Applicant: BASF AG

    Abstract: Riboflavin of the formula I I is prepared by condensation of a 4,5-dimethyl-N-(D)-ribityl-2-phenylazoaniline of the formula II II where X is H, -Cl, -NO2 or -CH3 in the o- or p-position, with barbituric acid of the formula III III in the presence of an acidic condensing agent in an inert organic solvent by an improved process in which the reaction is carried out in an aliphatic diol or triol derivative of the general formula IV (IV) where R1 is H or CH3, R2 is H or CH3- or, when n is 0, is CH3-CO-O-CH2-, R3 is CH3-, C2H5- or CH3-, R4 is CH3-CO-, or is H when R3 is CH3- or C2H5-, and n is 0 or 2, preferably 0, having a boiling point of 80 DEG -180 DEG C., or in a mixture of these as a solvent. In this process, the riboflavin is obtained in particularly pure form and in very good yields.

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