Cu2O−ZnO nanocatalyst has been successfully employed for the [3+2] cycloaddition reaction of propargyl ester with in situ generated nitrile oxide from aromatic hydroximyl chlorides under base‐free and mild temperature conditions for the regioselective synthesis of 3, 5‐disubstituted isoxazoles at a low loading of catalyst. The catalyst can be reused in further catalytic reactions up to five cycles without significant loss in its catalytic activity. The catalyst was characterized by using powder XRD, TEM, SEM and EDS. This developed methodology has advantages such as simplicity, excellent yields, shorter reaction time, and excellent functional group compatibility. [ABSTRACT FROM AUTHOR]