Alloying nanoparticle is a method to adjust the surface properties of catalysts so as to enhance catalytic performances of them and they usually exhibit outstanding characteristics which are disparate from monometallic nanoparticles. In this regard, a bimetallic catalyst based on sliver and cobalt nanoparticles incorporated in the structure of hierarchical ZSM-5 (Hi-ZSM-5) was produced. This novel catalyst was simply produced through simultaneous chemical reduction of silver and cobalt ions in the presence of Hi-ZSM-5. The solid support (Hi-ZSM-5) has played a highly crucial part in this catalyst because it offers a high surface area for deposition of nanoparticles as active sites and facilitates diffusion of reactants by its mesopores. The catalytic aspects of AgÀ Co/Hi-ZSM-5 were examined in A 3 coupling reaction of amine, aldehyde, acetylene in water media and impacts of different reaction parameters were extensively investigated. Outperforming both monometallic counterparts, the catalyst was found highly selective, stable and recoverable in the reaction and it did not show any sign of chemical or morphological alterations after 5 runs. The chemical composition and morphological properties of the catalyst were evaluated by XRD, BET, SEM-EDS, TEM, DRS-UV and ICP-AES techniques.