Nitrogen-containing heterocycles have attracted attention for the development of chemicals because of their many types, high physiological activities, and ease of synthesis. Aphids are severe pests found worldwide that cause serious losses in crop yield and quality every year. In this study, a series of novel dienolone thiazole derivatives were synthesized using dienolone acetate as the parent molecule. The synthesis involved bromination, Hantzsch reaction, esterification, deprotection, and other reactions. The structure of the compounds was determined using proton and carbon-13 nuclear magnetic resonance, high-resolution mass spectrometry, and single-crystal diffraction. The synthesized compounds exhibited excellent insecticidal activities against five species of aphids, including