Three distyryl-containing compounds, namely, 2-((cyanomethyl)thio)-4,6-distyrylnicotinonitrile (2), 3-amino-4,6-distyrylthieno[2,3-b]pyridine-2-carbonitrile (3) and 2-((2-cyanoethyl)thio)-4,6-distyrylnicotinonitrile (4) have been prepared and characterized by elemental and spectroscopic analyses. The three compounds contain the pyridine moiety and are considered neonicotinoids analogues. Because neonicotinoids were considered the most effective pesticides, the biological activity of the distyryl-containing compounds as potential insecticides against cowpea aphid, Aphis craccivora Koch was evaluated. The agricultural bioactivity results of these compounds showed that the insecticidal activity varied from good to moderate against cowpea aphid insects.