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Comb-shaped graft copolymers with poly(methyl methacrylate) as a handle were synthesized by the macromonomer technique in two steps. First, polytetrahydrofuran acrylate (A-PTHF), prepared by the living cationic ring-opening polymerization of tetrahydrofuran, underwent homopolymerization with 1-(ethoxycarbonyl)prop-1-yl dithiobenzoate as an initiator under ⁶⁰Co γ irradiation at room temperature; Second, the handle of the comb-shaped copolymers was prepared by the block copolymerization of methyl methacrylate with P(A-PTHF) as a macroinitiator under ⁶⁰Co γ irradiation. The two-step polymerizations were proved to be controlled with the following evidence: the straight line of ln[M]0/[M] versus the polymerization time, the linear increase in the number-average molecular weight with the conversion, and the relatively narrow molecular weight distribution. The structures of the P(A-PTHF) and final comb-shaped copolymers were characterized by ¹H NMR spectroscopy and gel permeation chromatography. © 2002 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 40: 3367–3378, 2002