New Schiff bases were synthesized by condensation of methyl-5-(furan-2-yl)-5-oxopentanoate, methyl-4(furan-2-yl)-4-oxobutanoate, methyl-5-(thiophene-2-yl)-5-oxopentanoate, and methyl-4-(thiophene-2-yl)-4-oxobutanoate with p-anisidine and n-butylamine. The structures of these synthesized compounds were clarified on the basis of elemental analysis, IR, H-1 NMR, C-13 NMR, and GC-MS spectroscopic techniques. In addition, antioxidant activity of the synthesized compounds was evaluated on the basis of DPPH radical.