From high silica zeolites,TiO2 powder and HClO4,Ti-M molecular sieves through isomorphous replacement of Al by Ti in zeolite M were successfully synthesized with to hydrothermal procedure.The sample were charactericed using FT-IR and UV-Vis.The results confirm that the titanium atoms are incorporated in the framework of M molecular sieves and indicate that there are indeed framework Ti species in the M molecular sieves.Ammoximation of cyclohexamone was selected as a probe reaction.The results prove that Ti-M molecular sieves exhibit good catalytic behavior in the reaction of ammoximation of cyclohexamone.