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A poly(styrene-b-isobutylene-b-styrene) triblock copolymer has been prepared by a two-step process. Polyisobutylene with Mn= 6600 and Mw/Mn= 1.12 functionalized with phenol at both ends was reacted with 2-bromopropionyl chloride to form a macroinitioator for atom transfer radical polymerization (ATRP). The synthesized difunctional PIB macroinitiator was subsequently heated with styrene xylene solution in the second step to 110C under conditions for ATRP using the copper coordination complex CuBr/bipyridine. Both the macroinitiator and the triblock copolymer were characterized by 1H NMR and SEC. The triblock copolymer with around 25% polystyrene was found to have a narrow molecular weight distribution of 1.20.