In-situ treatment of pyridine-2,3-dicarboxylic acid esters...

C - Chemistry – Metallurgy – 07 – D

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C07D 213/803 (2006.01) C07D 213/80 (2006.01)

Patent

CA 2530110

A method for the in-situ treatment of a pyridine-2,3-dicarboxylic acid ester with an oxidizing agent, such as hydrogen peroxide, to improve product quality is provided. The method for the in-situ removal of impurities from a saponified solution of pyridine-2,3-dicarblxylic acid ester comprises the steps of providing a solution of pyridine-2,3-dicarboxylic acid ester, saponifying the solution with a base to form the corresponding pyridine-2,3- dicarboxylic acid salt, reacting the solution with an oxidizing agent in an amount effective to remove impurities, acidifying the solution with an acid to convert the pyridine-2,3-dicarboxylic acid into the corresponding pyridine-2,3- dicarboxylic acid, and collecting a purified solution comprising pyridine-2,3- dicarboxylic acid. Further provided is a method for the preparation of herbicidal 2-(2-imidazolin-2-yl)nicotinic acids, esters, and salts by using a pyridine-2,3-dicarboxylic acid salt prepared by the above method as an intermediate.

L'invention concerne une méthode pour le traitement <i>in situ</i> d'un ester d'acide pyridine-2,3-dicarboxylique, à l'aide d'un agent oxydant, notamment du peroxyde d'hydrogène, pour améliorer la qualité du produit. La méthode destinée à retirer <i>in situ</i> des impuretés d'une solution saponifiée d'ester d'acide pyridine-2,3-dicarboxylique, comprend les étapes consistant à : fournir une solution d'ester d'acide de pyridine-2,3-dicarboxylique, saponifier la solution au moyen d'une base pour former le sel d'acide de pyridine-2,3-dicarboxylique correspondant, faire réagir la solution avec un agent oxydant dans une quantité efficace pour retirer des impuretés, acidifier la solution au moyen d'un acide pour convertir l'acide pyridine-2,3-dicarboxylique en acide pyridine-2,3-dicarboxylique correspondant, et recueillir une solution purifiée comprenant de l'acide pyridine-2,3-dicarboxylique. L'invention concerne également une méthode pour la préparation d'acides 2-(2-imidazolin-2-yl)nicotinique herbicides, d'esters et de sels associés, au moyen d'un sel d'acide de pyridine-2,3-dicarboxylique préparé par la méthode susmentionnée, en tant qu'intermédiaire.

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