In our present study, we evaluated insecticidal activities of substituted 1,3-diyenes (or) alkyne dimers. 1,3-diyenes were prepared by oxidative coupling in presence of Cu (I) catalytic system. All the compounds showed moderate and good insecticidal activity comparing to their standard drug Chloropyrifos. Compounds 2d and 2f were showed potential insecticidal activity compared to Chloropyrifos.