Abstract 3‐Substituted‐2‐acylaminoindazoles 2 were prepared via oxidative cyclization of o ‐aminoaryl ketone acylhydrazones 1 with iodosobenzene diacetate. Their electron ionization mass spectra were recorded and in addition to the molecular ions show common fragmentation pathways corresponding to the [M‐N 2 ] + , [M‐NHCOX] + and [M‐COX] + ions, with some influence on the skeletal fragmentation by different substituents.