The ACS Guidelines for bachelor's degrees in chemistry call for the curriculum to include polymer chemistry principles and the synthesis of different classes of macromolecules. Organic chemistry can provide an important introduction to polymer chemistry principles, and photochemically induced radical polymerization is one method for generating polymers that is well suited to be explored in this course. The development and implementation of an experiment for undergraduate organic chemistry laboratory in which students explore both photochemistry and radical chemistry by synthesizing cross-linked polymers via photopolymerization is reported. An inquiry design is used to introduce polymerization reactions, and students learn about air-sensitive lab techniques. Students must pool their data to explain how molecular structure affects the physical properties of a macroscopic material.