In continuation of our earlier work [1], we report a series of 2-(substituted phenyl)azo-4,6-diacetylresorcinol derivatives (I-VI) synthesized by diazotisation of substituted aniline followed by coupling with 4,6- diacetylresorcinol. All the synthesized compounds have been characterized by elemental analysis, IR, 1H NMR, 13C NMR and mass spectral analysis. In general azo resorcinol compounds can exist in azo hydrazone tautomeric forms. But in our study, all the spectral data show that 2-(substituted phenyl)azo-4,6-diacetylresorcinol derivatives (I-VI) exist in the azo form. Besides, In vitro antimicrobial activity of all the synthesized compounds has been evaluated against four strains of bacteria viz., Escherichia coli, Proteus vulgaris , Vibrio cholera and Salmonella typhi and two fungi viz., Aspergillus niger and Candida albicans. The study showed that all the synthesised compounds have potent activity.