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A discovery-based experiment highlighting the use of renewable starting materials to synthesize triblock polymers was developed and successfully implemented in our introductory organic chemistry laboratory course. Green chemistry principles applied in this experiment include the use of renewable feedstocks, minimal/green solvents, and design for degradation. Groups of students are tasked with synthesizing polymers of different compositions so that comparisons can be made of their mechanical properties. ¹H NMR analysis allows estimation of the overall molecular weight and quantification of the polymer blocks incorporated. The experiment serves to share modern state-of-the art technologies in sustainable polymers and addresses the ACS Committee on Professional Training’s accreditation guidelines to include synthetic polymers and macromolecules in the chemistry curriculum.