Herein, the design, synthesis, and characterization of four novel galloyloxadiazole hybrids are described. Compounds were evaluated in vitro as antioxidant agents by DPPH assay in comparison with reference antioxidants (ascorbic acid and butylated hydroxytoluene (BHT)) (scavenging of free radical 2,2-diphenyl-1-picrylhydrazyl DPPH). It was found that, interestingly, all compounds showed very strong antioxidant activity, even more than the water-soluble ascorbic acid. Such strong activity is related to the gallic acid moiety, as it has three dissociable OH groups via hydrogen atom transfer. The overall results suggest that these compounds could, potentially, be further modified for the formation of more potent antioxidant, and more biological studies are under investigation. These studies should be conducted in the following study.