The control of insect pests and invasive weeds has become more species-selective because of activity-guided isolation, structure elucidation, and total synthesis of naturally produced substances with important biological activities. Examples of isolated compounds include insect pheromones, antifeedants, and prostaglandins, as well as growth regulators for plants and insects. Synthetic analogues of natural substances have been prepared to explore the relationships between chemical structure and observed biological activity. Recent scientific advances have resulted from better methods for the chemical synthesis of target compounds and better analytical methods. The capability of analytical instrumentation continues to advance rapidly, enabling new insights.