Process for the preparation of intermediates useful in the...

C - Chemistry – Metallurgy – 07 – D

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C07D 501/04 (2006.01) C07D 501/00 (2006.01) C07D 501/18 (2006.01) C07D 501/22 (2006.01) C25B 3/04 (2006.01)

Patent

CA 2206226

A process is described for preparing 3-exomethylene cephalosporanic acid derivatives for use in the synthesis of cephalosporin antibiotics such as ceftibuten. The process comprises electrochemical reduction of a compound of formula (IV), wherein: R3 is CH3C(O)-; a is an optional sulfoxide group; n is 2 or 3; R1 is H and R is H or NHR2, where R2 is H or a protecting group selected from C6H5CH2OC(O)-, C6H5C(O)- or C1-C6 alkoxy-C(O)-; or wherein R and R1 together with the carbon atom to which they are attached comprise -C(O)-, and produces the desired 3-exomethylene compounds with low levels of the corresponding 3-methyl tautomers.

Procédé de préparation de dérivés d'acide 3-exométhylène céphalosporanique utilisé dans la synthèse des antibiotiques céphalosporines tels que le ceftibutène. Le procédé comprend la réduction électrochimique d'un composé de la formule (IV), dans laquelle: R?3¿ représente CH?3¿C(O)-; (a) représente un groupe oxyde sulfonique optionnel; n représente 2 ou 3; R?1¿ représente H et R représente H ou NHR?2¿, où R?2¿ représente H ou un groupe protecteur choisi parmi C¿6?H¿5?CH¿2?OC(O)-, C¿6?H¿5?C(O)- ou alcoxy C¿1?-C¿6?-C(O)-; ou dans laquelle R ainsi que R?1¿ avec l'atome de carbone auquel ils sont fixés comprennent -C(O)-. Le procédé produit les composés 3-exométhylène voulus à de faibles niveaux de tautomères 3-méthyle correspondants.

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