This course provides a comprehensive understanding of macromolecule synthesis, growth quantification, and the translation of synthetic strategies into functional materials. Students explore all major polymerization methods; step-growth, free-radical (bulk, solution, suspension, emulsion, controlled/living), ionic, coordination, ring-opening, and copolymerization; while applying kinetic and thermodynamic models (Carothers, radical rate laws, Mayo–Lewis, gelation theory) to predict conversion, molecular weight distribution, and architecture. Structure–property relationships including glass-transition behavior, crystallinity, crosslink density, and network formation are integrated throughout reaction design discussions. The course emphasizes converting mechanistic insights into practical process conditions that achieve targeted thermal, mechanical, or functional performance. Students develop hands-on expertise through integrated laboratory and analysis modules, synthesizing representative polymers, monitoring real-time reactions, and characterizing products using modern analytical techniques. Upon completion participants can formulate synthetic pathways, manipulate reaction variables to control macromolecular architecture, and connect chemical structure to end-use properties, essential skills for advanced materials science and nano-engineering research.