A series of 4, 6-diacetyl-1, 3-di(substituted-phenyl carbonyloxy)benzenes or diesters (2a-f) were prepared and screened for in vitro antibacterial and antifungal activities. 1, 1´-(4,6-Dihydroxy-1, 3-phenylene)diethanone (1) was treated with different aromatic acids in dry pyridine in presence of phosphorous oxychloride to obtain the diesters (2a-f). The structures of the synthesized compounds were established on modern analytical techniques. The antimicrobial activity (minimum inhibitory concentration; MIC) of the title compounds was determined against some selected bacterial and fungal strains. The compounds showed appreciable antimicrobial activity against the tested microbes. Presence of halogen group(s) was found to increase the antimicrobial activity of the diesters.