A series of new 4-(3,4dimethoxyphenethyl)-3,5-akyl/aryl-4H-1,2,4-triazoles (3a-g) were obtained by reaction of ethyl N'-(alkylidene/arylidene) hydrazonate (1) and 2-(3,4-dimethoxy phenyl) ethanamine (2). Compounds 4d, e, and g were synthesized from the reaction of corresponding compounds 3d, e, and g with BBr3, respectively. The 10 new compounds synthesized were characterized by elemental analyses, IR, H-1-NMR, and C-13-NMR spectral data. The structure of compound 3g was inferred through IR, H-1-, C-13-NMR, elemental analyses, and X-ray spectral techniques. In addition, the newly synthesized chemicals were screened for their antioxidant properties. Among the chemicals tested, 4d, e, and g exhibited the highest degree of antioxidant activity.