Herein, we demonstrate the ultrasonic‐assisted synthesis of Palladium/Copper nanoalloy supported on carbon nanotubes (PdCu/CNT) towards the electro‐oxidation of methanol and ethylene glycol using Triton X‐100 as a stabilizer. Structural and morphological analysis manifests the formation of PdCu nanoalloy on the surface of CNTs. For the electrochemical comparison, PdCu on Vulcan carbon (PdCu/VC) also synthesized in the same procedure and characterized thoroughly. The electrochemical evaluations of the PdCu/CNT reveal the better mass activity of 1021.6 mA mg[pd]−1 which is 1.6‐fold higher than PdCu/VC and 5.9 times advanced than commercial Pd/C catalysts towards methanol electrooxidation. Also, for electrooxidation of ethylene glycol, the mass activity of the PdCu/CNT is more of about 1219.8 mA mg[pd]−1 which is around 1.7 times enhanced than PdCu/VC and 4.1 times improved than commercial Pd/C catalysts. Furthermore, sonochemically prepared PdCu/CNT provides improved stability up to 3600s in both methanol and ethylene glycol oxidation reactions. The accredited activity enhancement due to its unique construction of zero‐dimensional structured PdCu nanoalloy with one‐dimensional CNTs and modified electronic effect of Pd on it.