In the present study, a series of substituted Semicarbazones were synthesized, characterization and evaluated for their antimicrobial activity. A series of substituted semicarbazones were synthesized from substituted phenyl urea followed by hydrazine hydrate gave good yield of Semicarbazide, Which were further on treatment with appropriate substituted acetophenones yielded the semicarbazones (SC01-SC04). All the synthesized compounds were characterized on the basis of their IR, 1H and 13C NMR studies. The antimicrobial activity of all the compounds (SC01-SC04) showed significant activity against all the bacteria and fungus.