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Two series of vanadium‐containing oxynitrides VMON (M=Al or Zr, 0.1<V/M<0.5) were characterized by a variety of methods, also under reaction conditions, and tested as catalysts for the ammoxidation of 3‐picoline. Markedly higher space–time yields of 3‐cyanopyridine have been obtained for both types of catalysts in comparison to the best‐known mixed oxide catalysts, although selectivities were lower. VZrON catalysts are more active but less selective than VAlON, which might be due to higher V site agglomeration and higher mean V valence in working VZrON catalysts. The higher selectivity of VAlON catalysts results from the reversible incorporation of N in VNAl surface moieties, whereas this is widely suppressed in VZrON samples, in which the majority of N is incorporated within the bulk.

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