In this study, the oxidation of diarylalkynes, which were prepared from benzaldehyde through three synthetic steps, with PdCl2/CrO3/H2O was described. We found the multiple-methoxy substituted diarylalkynes can be oxidized by the oxidation system to give corresponding diaryldike -tones (benzyls) in excellent yields. However the less or no substituted diarylalkynes gave diaryldiketones in low yield or in trace amount.