(E)-4-oxo-2-alkenals are defensive secretions (allomones) produced by true bugs and also serve as important pheromone components in various insect species. Despite numerous reports detailing their synthesis, significant challenges remain regarding their stability and yield percentages, which limit practical applications. In this study, we synthesized three specific (E)-4-oxo-2-alkenals: (E)-4-oxohex-2-enal, (E)-4-oxooct-2-enal, and (E)-4-oxodec-2-enal by modifying an existing method. Stabilities of these compounds were evaluated under two different storage conditions: room temperature and refrigeration. After a streamlined one-step synthesis, these (E)-4-oxo-2-alkenals were obtained with high purity (≥97%), confirmed by GC-MS analysis. Our stability testing shows that when stored in a refrigerator, these compounds remain the original purities for at least three months. In contrast, their stabilities at room temperature extend to two months while maintaining purities of ≥85%. These promising stability profiles not only highlight the feasibility of using these compounds in practical applications but also emphasize their potential role in advancing pest management strategies in the field.