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A new class of light-responsive supramolecular amphiphilic block copolymers (BCs) based on the association through multiple H-bonding between 4-isobutyloxyazobenzene motifs and 2,6-diacylaminepyridine units is reported. Block copolymers containing 2,6-diacylaminopyridine side units, as hydrophobic block, and poly(ethylene glycol), as a hydrophilic segment, were functionalized with either a carboxylic acid azodendron, via double H-bonding, or a thymine azobenzene, via triple H-bonding. The structural and thermal characterization of these supramolecular azo-copolymers in bulk and solution is presented. The work emphasizes the self-assembly of these supramolecular polymers in water and the study of their UV-light responsive properties by UV-vis spectroscopy, dynamic light scattering (DLS), transmission electron microscopy (TEM), and synchrotron small-angle X-ray (SAXS). The present noncovalent postpolymerization functionalization strategy has provided stable self-assemblies in water with light responsive properties that can be used to load and trigger the delivery of small fluorescent molecules.This work was supported by the MINECO, Spain, under Projects MAT2014-59187-R and MAT2014-55205-P, FEDER funding, and Aragon Government. A.C. acknowledges MINECO for his Ph.D. grant. A.M.-F. expresses thanks for the financial support of the Generalitat Valenciana for his APOSTD/2013/054 grant.Peer Reviewe

Light-Responsive Self-Assembled Materials by Supramolecular Post-Functionalization via Hydrogen Bonding of Amphiphilic Block Copolymers