Two new series of azo-azomethine compounds based on sulfathiazole and sulfadiazine were synthesized. Condensation of sulfathiazole diazonium salt and sulfadiazine diazonium salt with 3-ethoxy-4-hydroxy benzaldehyde. These new azo compounds were reacted with sulfathiazole, sulfadiazine,3-hydroxy aniline, 2-amino-4,6-dimethyl pyridine, and 4-bromoaniline respectively, to form the new azo-azomethine compounds. All compounds were characterized by CHN analysis, IR, 1H NMR, and mass spectroscopic data. Antibacterial activities were studied for these compounds in‐vitro and showed some promising activity against Escherichia coli and Staphylococcus aureus. The antifungal activity against Candida albicans and Aspergillus niger was studied and showed good activity. The antioxidant activity was evaluated by using antioxidant tests via the free radical scavenging (DPPH) method and showed good antioxidant activities.