Multiarm star triblock terpolymers were obtained by using two different click reactions sequentially: Cu(I) catalyzed azide–alkyne and Diels–Alder. The synthetic strategy is described as follows: (poly(methyl methacrylate))n-(polystyrene)m-poly(divinyl benzene)) ((PMMA)n-(PS)m-polyDVB) multiarm star diblock copolymer was first obtained from an azide–alkyne click reaction of (alkyne-PS)m-polyDVB multiarm star polymer with α-anthracene-ω-azide PMMA (anth-PMMA-N3), followed by a Diels–Alder click reaction of the anthracene groups at the star periphery with α-maleimide poly (tert-butyl acrylate) (PtBA-MI) or α-maleimide poly(ethylene glycol) (PEG-MI) leading to target (PtBA)k-(PMMA)n-(PS)m-polyDVB and (PEG)p-(PMMA)n-(PS)m-polyDVB multiarm star triblock terpolymers. The hydrodynamic diameter of individual multiarm star triblock terpolymers were measured by dynamic light scattering (DLS) to be ∼24–27 nm in consistent with the atomic force microscopy (AFM) images on silicon substrates. © 2010 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 48: 1557–1564, 2010
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