Process for preparing alkyl...

C - Chemistry – Metallurgy – 07 – C

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C07C 67/343 (2006.01) C07C 69/72 (2006.01)

Patent

CA 2715668

A process for preparing alkyl 2--alkoxymethylene-4,4-difluoro-3-oxobutyrates (VI) where R is methyl or ethyl, from crude reaction mixtures of alkyl 4,4-difluoroacetoacetates (I) by a) reacting alkyl acetate (II), RO M alkoxide (III), where M is a sodium or potassium ion, and alkyl difluoroacetate (IV), without additional solvent to form an enolate (V), b) releasing the corresponding alkyl 4,4-difluoroacetoacetate (I) from the enolate (V) by means of acid, c) removing the salt formed from cation M and acid anion as a solid and d) converting (I), without isolation from the crude reaction mixture, to the alkyl 2-alkoxymethylene-4,4-difluoro-3-oxobutyrate (VI), and the use of (VI) for preparing 1-methyl-3-difluo- romethyl-pyrazol-3-ylcarboxyates (VII).

L'invention porte sur un procédé de préparation de 2-alcoxyméthylène-4,4-difluoro-3-oxobutyrates d'alkyle (VI) où R représente méthyle ou éthyle, à partir de mélanges réactionnels bruts de 4,4-difluoroacétoacétates d'alkyle (I) par a) réaction d'acétate d'alkyle (II), d'alcoolate RO M (III), où M représente un ion sodium ou potassium et de difluoroacétate d'alkyle (IV), sans solvant supplémentaire pour former un énolate (V), b) libération du 4,4-difluoroacétoacétate d'alkyle (I) correspondant à partir de l'énolate (V) au moyen d'un acide, c) élimination du sel formé à partir du cation M et de l'anion acide sous la forme d'un solide, et d) conversion de (I), sans isolement à partir du mélange réactionnel brut, en le 2-alcoxyméthylène-4,4-difluoro-3-oxobutyrate d'alkyle (VI). L'invention porte également sur l'utilisation de (VI) pour la préparation de carboxylates de 1-méthyl-3-difluorométhyl-pyrazol-3-yle (VII).

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