Nanoscale microreactor containing “3,10-dialkyl-dibenzo-1,3,5,8,10,12-hexaazacyclotetradecane, [Ni(R 2 Bzo 2 [14]aneN 6 )] 2+ , R=H, Me, Et, Bu and benzyl” was successfully prepared by the in situ one-pot template synthesis (IOPTS) of formaldehyde and 1,2-phenylenediamine (1,2-phen) with alkyl and benzyl amine within the nanodimensional pores of zeolite-Y. The new host–guest nanocomposite materials “[Ni(R 2 Bzo 2 [14]aneN 6 )] 2+ –NaY” were characterized by several techniques: chemical analysis and spectroscopic methods (FT-IR, UV/Vis, XRD, BET, DRS) and then were used for oxidation of cyclohexene with molecular oxygen.