In this report, we present double-hydrophilic block glycopolymers of poly(2-hydroxyethyl methacrylate)-b-poly(2-(β-glucosyloxy)ethyl methacrylate) (PHEMA-b-PGEMA) and amphiphilic block glycopolymers of poly(ethyl methacrylate)-b-PGEMA (PEMA-b-PGEMA) synthesized via reversible addition–fragmentation chain transfer (RAFT) polymerization. The block glycopolymers were prepared in two compositions of P(H)EMA macro-chain transfer agents (CTAs) and similar molecular weights of PGEMA. Structural analysis of the resulting polymers as well as the conversion of (H)EMA and GEMA monomers were determined by 1H NMR spectroscopy. Size exclusion chromatography measurements confirmed both P(H)EMA macro-CTAs and block glycopolymers had a low dispersity (Đ ≤ 1.5). The synthesized block glycopolymers had a degree of polymerization and a molecular weight up to 222 and 45.3 kg mol–1, respectively. Both block glycopolymers self-assembled into micellar structures in aqueous solutions as characterized by fluorescence spectroscopy, ultraviolet–visible spectroscopy, and dynamic light scattering experiments.

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