Process for the preparation of 2,3-pyridinedicarboxylic acids
    1.
    发明授权
    Process for the preparation of 2,3-pyridinedicarboxylic acids 失效
    2,3-吡啶二羧酸的制备方法

    公开(公告)号:US06395903B1

    公开(公告)日:2002-05-28

    申请号:US09569057

    申请日:2000-05-10

    IPC分类号: C07D21380

    CPC分类号: C07D213/80

    摘要: Process for the preparation of pure 2,3-pyridinedicarboxylic acids of the formula I which are substituted in position 4 and/or 5 and/or 6 by R1, where R1 is hydrogen, C1-C4 alkyl, C1-C4 alkoxy, C1-C4 alkoxy-C1-C4 alkyl, halogen, hydroxyl or nitro, from quinolines of the formula II in which R1 is as defined above, and which are substituted in position 6 and/or 7 by R2, where R2 is hydrogen, C1-C4 alkyl, C1-C4 alkoxy, C1-C4 alkoxy-C1-C4 alkyl, halogen, hydroxyl, nitro or amino, which are reacted in the first step in aqueous sulfuric acid or nitric acid solution with ozone in the ratio of from 1:2 to 1:3 at temperatures from 0 to +50° C., and the resulting peroxide solution is then reacted at temperatures of from +0 to +100° C. in the presence of 0.5-4.0 mol of oxidizing agent per mole of ozonolysis product formed, after which the pH of the reaction solution is adjusted to 0.2 to 3, the mixture is cooled to 0 to 30° C., and the precipitated pyridinedicarboxylic acid is isolated.

    摘要翻译: 制备式Ⅰ的纯的2,3-吡啶二羧酸的方法,其中R1是氢,C1-C4烷基,C1-C4烷氧基,C1-C4烷基, 烷氧基-C 1 -C 4烷基,卤素,羟基或硝基,其中R 1如上定义,并且其中R 2为氢,C 1 -C 4烷基,C 1 -C 4烷基, C 1 -C 4烷氧基,C 1 -C 4烷氧基-C 1 -C 4烷基,卤素,羟基,硝基或氨基,它们在第一步中在硫酸水溶液或硝酸溶液中与臭氧按1:2比1反应 :3,在0至+ 50℃的温度下,然后将所得过氧化物溶液在+ 0至+ 100℃的温度下在每摩尔臭氧分解产物0.5-4.0摩尔氧化剂存在下反应 之后,将反应溶液的pH调节至0.2〜3,将混合物冷却至0〜30℃,分离析出的吡啶二甲酸。