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Motivated by the prominent catalytic performance and durability of nanoalloy catalysts, the Pd-based bimetallic nanoalloy catalysts were prepared using an aqueous reduction method. The Fe-Pd bimetallic nanoalloy catalyst (nano-Fe/Pd) demonstrated 98.4% yield and 99.7% selectivity for the unsaturated 1,4-dicarboxylic acid diesters. Moreover, the inductively coupled plasma (ICP) analysis shows that the Pd leaching of the catalyst can be effectively suppressed by alloying Fe atoms into the Pd crystal lattice for acetylene dicarbonylation. The detailed catalyst structure and morphology characterization demonstrate that introducing Fe into the Pd nanoparticles tunes the electronic–geometrical properties of the catalyst. Theoretical calculations indicate that the electrons of Fe transfer to Pd in the nano-Fe/Pd catalyst, enhancing activation of the C≡C bond in acetylene and weakening CO absorption capacity on catalyst surfaces. Alloying Fe into the Pd nanocatalyst effectively inhibits active metal leaching and improves catalyst activity and stability under high-pressure CO reactions. [ABSTRACT FROM AUTHOR]