Process for preparing pyridinamines and novel polymorphs...

C - Chemistry – Metallurgy – 07 – D

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Details

C07D 213/74 (2006.01) A01N 43/40 (2006.01) A01P 1/00 (2006.01) A01P 3/00 (2006.01) A01P 7/00 (2006.01) A61K 31/44 (2006.01) A61P 31/04 (2006.01) A61P 31/10 (2006.01)

Patent

CA 2628475

The present invention relates to an improved process for the synthesis and purification of 3-chloro-N-(3-chloro-5-trifluoromethyl-2-pyridyl)-a,a,a- trifluoro-2,6-dinitro-p-toluidine (fluazinam) and other pyridinamines, which implements methyl isobutyl ketone (MIBK) as the reaction solvent. The process of the invention overcomes the drawbacks of prior art methods, by reducing the side reactions such as hydrolysis, eliminating the need for difficult and labor-intensive purification methods, and providing pure products in higher yields. The present invention relates to novel crystalline polymorphic forms fluazinam, and to mixtures of the polymorphs. The present invention also provides methods for preparing the novel polymorphs, as well as pharmaceutical compositions comprising same, and methods of using the polymorphs as pesticidal agents for combating noxious living organisms on agricultural and horticultural crops.

L'invention concerne un procédé amélioré de synthèse et de purification de 3-chloro-N-(3-chloro-5-trifluorométhyl-2-pyridyl)-.alpha.,.alpha.,.alpha.-trifluoro-2,6-dinitro-p-toluidine (fluaziname) et d'autres pyridinamines, qui met en oeuvre le méthylisobutylcétone (MIBK) comme solvant de réaction. Ledit procédé permet de surmonter les insuffisances des procédés de la technique actuel, car il réduit les réactions secondaires telles que l'hydrolyse, élimine la nécessité de procédés de purification à la fois difficiles et exigeants en main d'oeuvre, et fournit des produits purs en plus grandes quantités. L'invention concerne de nouvelles formes polymorphiques cristallines de fluaziname, ainsi que des mélanges des polymorphes. Elle concerne également des procédés permettant de préparer les nouveaux polymorphes, ainsi que des compositions pharmaceutiques les comprenant, et des procédés d'utilisation des polymorphes comme agents pesticides destinés à combattre des organismes vivants nuisibles des récoltes agricoles et horticoles.

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