Abstract Ethenylbenzene-terminated poly(2-acetoxyethyl methacrylate) macromonomer, 2-methyl-2-propenoate-terminated poly (2-acetoxyethyl methacrylate) macromonomer, and 2-methyl-2-propenoate-terminated poly (methyl methacrylate) macromonomer were synthesized. The number-average molecular weight of the macromonomers could be controlled by adjusting the feed composition. Comb-type polymers and graft copolymers were prepared by homopolymerization and copolymerization of macromonomer with comonomer. Unreacted macromonomer in the resulting polymers could be determined by calculating the areas of the macromonomer peaks on gel permeation chromatograms (GPC).