A multistep experiment for a synthesis laboratory course that incorporates topics in organic synthesis, chemical analysis, and instrumental analysis was developed. Students prepared a tertiaryamine-functionalized polyacrylonitrile fiber (PAN[subscript T]F), and it was subsequently utilized as an immobilized catalyst in a three-component condensation reaction among an aromatic aldehyde, malononitrile, and a-naphthol in ethanol to synthesize substituted 2-amino-2-chromenes in one pot. The fiber catalyst exhibits the advantages of high yield, excellent recyclability and reusability, simple post-treatment, and environmental friendliness. Thus, students were able to apply the concept of green chemistry through catalysis. Moreover, this comprehensive experiment involves a number of unit operations, such as vacuum distillation, filtration, recrystallization, and acid-base titration, which can train the fundamental operation capability of students, and improve their experimental skills.