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The equilibrium constant, Kmodel, of iron‐mediated atom‐transfer radical polymerization (ATRP) is investigated for FeBr2/α‐bromoester model systems in the absence of monomer. Quantitative analysis is carried out in solution of either N‐methylpyrrolidin‐2‐one (NMP) or acetonitrile (MeCN) via high‐pressure online VIS/NIR spectroscopy monitoring the formation of the FeIII species. The reaction volume...