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The Cu(0)\/Cu(II) catalytic system allowed the controlled polymerization of <jats:italic>tert<\/jats:italic>\u2010butyl acrylate with narrow dispersity in less than an hour. Kinetic studies revealed that the initial catalyst ratio influences the polymerization time by means of an induction period that increases with the [Cu(II)]<jats:sub>0<\/jats:sub>\/[Cu(0)]<jats:sub>0<\/jats:sub> ratio. The effect of nitrogen purge and freeze\u2010pump\u2010thaw cycles was assessed, and both were found to be equally effective in the system deoxygenation. The synthesized polymers exhibited a high degree of chain\u2010end fidelity, as evidenced by the results of chain extension experiments. This makes the system interesting for the formation of block copolymers with cholesterol\u2010termination, broadening its range of applicability.<\/jats:p>","DOI":"10.1002\/pol.20250415","type":"journal-article","created":{"date-parts":[[2025,6,16]],"date-time":"2025-06-16T06:55:47Z","timestamp":1750056947000},"page":"3350-3357","update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Insights Into the Kinetics and Chain Extension in the Synthesis of Cholesterol\u2010Terminated Poly(<i>Tert<\/i>\u2010Butyl Acrylate) via Controlled Radical Polymerization"],"prefix":"10.1002","volume":"63","author":[{"ORCID":"https:\/\/orcid.org\/0000-0003-2510-8790","authenticated-orcid":false,"given":"Gina","family":"Tavares","sequence":"first","affiliation":[{"name":"CERES, Chemical Engineering and Renewable Resources for Sustainability, Department of Chemical Engineering University of Coimbra  Coimbra Portugal"},{"name":"CQM, Centro de 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