A tailored nanostructured CuO–ZnO/Al2O3 catalyst was obtained from nanocomposites via sonochemical route through core/shell assisted by reverse micelle synthesis. The as-synthesized nanocomposites consisted of Cu, Zn and Al domains coated by a lauric acid shell structure with controlled physicochemical properties. Combining these features, a porous CuO–ZnO/Al2O3 supported catalyst was obtained from CuZnAl@C nanocomposite, in which Cu and Zn oxide nanoparticles interacted quite strongly with alumina. In this study, a nanostructured CuO–ZnO/Al2O3 was applied to oxidize ethylbenzene in the presence of H2O2. Catalytic results further demonstrated that the nanostructured solid had ethylbenzene conversion superior to 20% and good selectivities to acetophenone, benzaldehyde and benzoic acid compared to a benchmark CuZnAl catalyst obtained by the sol-gel method. Display omitted •Tailored CuO–ZnO/Al2O3 catalyst obtained from CuZnAl@C nanocomposite.•Simple sonochemical route via core/shell assisted by reverse micelle synthesis.•Nuclei composed of Cu and Zn domains coated by a semi-crystalline lauric acid-based shell.•Highly dispersed CuO and ZnO on alumina converting ehtylbenzene.