Two new dioxomolybdenum (VI) complexes [MoO2 (acac) LL'] (I) and [MoO2L2L2"] (II) [L=OC (CH3) CHCOCH3, L'=NH2C6H4NH2, L"=NH2C6H3CH3NH2] with diamine o-Phenylenediamine (OPDA) and 4- Methyl-o-Phenylenediamine (4-Me-OPDA) ligands have been synthesized and characterized. Compounds (I) (61% yield) and (II) (62% yield) were obtained from the reactions of MoO2 (acac)2 [acac=acetyl acetonato] with 1 equiv. of OPDA and 4-Me-OPDA.1H, 13C NMR, IR spectral data indicated that the ligands acted as unidentate and structures of both compounds were six-coordinated. The dioxomolybdenum (VI) complexes (I) and (II) are efficient catalysts for oxidation of alcohols with H2O2 as an oxidant.