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ABSTRACT: A series of well-defined amphiphilic graft copoly-mers, containing hydrophilic poly(acrylic acid) backbone and hydrophobic poly(butyl acrylate) side chains, were synthesized by sequential reversible addition fragmentation chain transfer (RAFT) polymerization and atom transfer radical polymerization (ATRP) without any postpolymerization functionality modifica-tion followed by selective acidic hydrolysis of poly(tert-butyl acrylate) backbone. tert-Butyl 2-((2-bromopropanoyloxy)-methyl)-acrylate was first homopolymerized or copolymerized with tert-butyl acrylate by RAFT in a controlled way to give ATRP-initiation-group-containing homopolymers and copoly-mers with narrow molecular weight distributions (Mw/Mn < 1.20) and their reactivity ratios were determined by Fineman-Ross and Kelen-Tudos methods, respectively. The density of ATRP initiation group can be regulated by the feed ratio of th