The realization of polymer conjugate-based RNA delivery as a clinical modality requires the development and optimization of novel formulations. Although many literature examples of polymer conjugate-based SiRNA delivery systems exist, the protocols described herein represent a robust and facile way of screening any poly(amine)-based polymer system for SiRNA delivery. In this chapter, we describe the synthetic methods used to prepare poly(amide) polymers using a controlled polymerization method, as well as the preparation of the resulting targeted SiRNA polymer conjugates. In addition, detailed methods are provided for the characterization of the biodegradable poly(peptides) as well as the polymer conjugate that ensues.
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