Macromonomers as Well‐Defined Building Blocks in the Synthesis of Hybrid Octafunctional Star‐Shaped Poly(ethylene oxide)s

Abstract The present work addresses the synthesis and the molecular and structural characterization of soluble macromolecular architectures based on functional poly(ethylene oxide) (PEO)s and octafunctional silsesquioxanes. The synthesis of a series of functional PEOs by deactivation, decorated with allyl groups at one chain‐end, was considered first. PEO star‐shaped polymers were prepared by coupling via hydrosilylation of ω‐allyl PEOs with octakis(hydridodimethylsiloxy)octasilsesquioxane (HMe 2 SiOSiO 1.5 ) 8 (Q 8 M 8 H ), in the presence of a “Speier” catalyst. The products were characterized by SEC, 1 H NMR spectroscopy, light scattering, and MALDI–TOF MS to determine the molar masses and degree of functionalization. The star‐shaped PEOs (Q 8 M 8 PEO ) could be isolated from the raw reaction product and characterized. A functionalization close to the theoretical value was obtained.