Development of biologically active polymers is an active area of research due to their applications in varied and diverse fields of biomedical research: cell adhesion, tissue proliferation, and drug delivery. Recent advances in chemical modification allow fine-tuning of the properties of biomedical polymers to improve their applications: blood circulation half-life, stimuli-responsive degradation, site-specific targeting, drug loading, etc. In this article, convergent synthesis of polymerizable macromonomers bearing a site-specific ligand (RGD peptide) using a low molecular weight MA-poly(ethylene glycols) (PEGs) is presented. The method affords macromonomers useful as the starting materials to produce biomedical polymers. We found matrix assisted laser desorption/ionization mass spectromerty convenient in monitoring the conjugation process via step-by-step following of PEG modification. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014, 131, 40385.