Thiosemicarbazones exhibit various biological activities and have attracted considerable pharmaceutical interest. They have been evaluated over the last 50 years as antibacterial, antifungal, antiviral, antitubercular, antitumor and anticancer therapeutics. Studies have been conducted on compounds bearing-N=N- ,-N-C=S, and-CH=N-as pharmacophore. 5-[(3-Substitutedphenyl)diazenyl]-2-hydroxybenzaldehydeN-(3-Substitutedphenyl)thiosemicarba zones(3a-l) has been Synthesized by the condensation of

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... droxy 5-(substituted phenyl azo)benzaldehydes (1) and thiosemicarbazides (2). Purity of compounds were ascertained by Column chromatography and the structures were assigned on the basis of elemental analysis and spectral analysis. The synthesized compounds were screened for antimicrobial activities using Kirby-Bauer disc diffusion technique against two bacterial pathogens viz Bacillus anthresis (gram positive), Escherichia coli (gram negative) & two fungal pathogens Candida albicanes, Aspergillus niger. Chloramphenicol and fluconazole were used as standard drug respectively. The compounds exhibit moderate activity.