3-Miktoarm star copolymers, 3 mu-D2V, with two poly(dimethylsiloxane) (PDMS) and one poly(2-vinylpyridine) (P2VP) arm, were synthesized by using anionic polymerization-high vacuum techniques and (chloromethylphenylethyl)methyl dichlorosilane, heterofunctional linking agent, with two SiCl groups and one CH2Cl group. The synthetic strategy involves the selective reaction of the two -SiCl groups with PDMSOLi living chains, followed by reaction of the remaining chloromethyl group with P2VPLi. Combined molecular characterization results (size exclusion chromatography, membrane osmometry, and H-1 NMR spectroscopy) revealed a high degree of structural and compositional homogeneity. (c) 2005 Wiley Periodicals, Inc.