Rise of the mute assassin “carbon monoxide (CO)” levels impact all aerobic life. The elevated rates of CO concentration endure climatic and geographical characteristics that exacerbate air pollution. Herein, a simple approach for hydrothermal leaching (HyTL) of Al3TM‐Rh0.5 (Target material (TM)=Zr, V, Ce) and Al3TM (TM=Zr, V, Ce) intermetallic compounds produces leached products of ZrO2, VO2, and CeO2 with Rhodium (Rh) as an active component. The characterization result reveals the HyTL process and the presence of the active Rh element that elevated the performance of HyTL‐Al3Zr‐Rh0.5 towards CO conversion compared to other samples. Further, the cubic ZrO2 phase selectively forms after HyTL at 130 °C even though the formation of the cubic ZrO2 phase takes place at a high temperature. Moreover, the presence of Rh promotes higher catalytic activity in all the cases with low temperatures. The advancement in the present study towards the catalytic oxidation of CO over the hydrothermally leached ZrO2‐Rh nanocatalyst guarantees the perspective of the aggregation‐activation process.