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Knoevenagel condensation between aryl aldehyde derivatives with malononitrile was successfully achieved using commercially available Pd/AlO(OH) nanoparticles (0.5 wt% Pd) in an aqueous medium. All benzylidenemalononitrile (BMN) derivatives were obtained promptly (8‐60 min) with high selectivity and yields of over 99 % in a mixture of H2O/MeOH (v/v=1/2) at room temperature. Moreover, when benzoyl chloride derivatives were utilized instead of aryl aldehyde derivatives, medium amounts of the expected products were yielded. Before the reaction and after five reuses, characterization of the Pd/AlO(OH) nanoparticles was carried out via X‐ray diffraction and scanning electron microscopy analysis. The BMN derivative characterization was accomplished using the 1H NMR and 13C NMR spectra. In order to optimize the reaction conditions, the parametric effects of the solvent type and catalyst amount were examined. Consequently, the PdAlO(OH) NPs were used for the first time in the Knoevenagel condensation. A novel, practical and eco‐friendly process was developed for Knoevenagel condensation in the presence of Pd/AlO(OH) nanoparticles.

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