Hierarchical HY zeolite (Hie-Y) with a SiO2/Al2O3 molar ratio of 10 was successfully synthesized through sequential desilication-dealumination using NH4OH treatment. The combination of a weak alkaline media and surfactant cetyltrimethylammonium bromide (CTAB) not only facilitates the formation of mesoporosity but also preserves the zeolite structure. Metal oxide (CuO, MoO3) - hierarchical HY zeolite nanocomposites were prepared by one or a combination of 3 methods: 1) ion exchange, 2) precipitation, and 3) calcination. The obtained catalysts were characterized using XRD, FT-IR, FESEM, UV-Vis, EDS, and BET techniques. Hierarchical zeolite formation is accompanied by structure preservation, but based on the entering Cu in the zeolite porous, slight destruction is observed. The catalytic activity of the catalysts was investigated in the oxidative desulfurization (ODS) reaction. Several parameters, including temperature, catalyst amount, DBT concentration, and reaction time, were evaluated in ODS using the Taguchi Design of Experiments. Catalytic activity order obtained: Y < Hie-Y < Hie-Y /CuO-Hie < MoO3-Hie < CuO/MoO3-Hie-Y. Results indicate an activity increase for the CuO/MoO3-Hie-Y hierarchical structure owing to synergistic effects of secondary mesoporosity and metal oxides. The catalyst was recoverable and reused for five consecutive runs with preservation of catalytic activity.