A convenient route for the synthesis of a diblock copolymers made of a thermosensitive poly(2-isopropyl-2-oxazoline) (LCST) and a pH sensitive poly(L-glutamate) was analyzed. The cationic polymerization of oxazolines was carried out over the controlled radical or anionic polymerization of acrylamides/acrylates because the products can be of higher functionality. H NMR measurements were carried out at room temperature on a Bruker DPX-400 spectrometer operating at 400.1 MHz and FT-IR spectroscopy was performed on a BioRad 6000 FT-IR spectrometer equipped with a single reflection diamond ATR.The target block copolymer was made through a combination of a cationic ring-opening polymerization of 2-isopropyl-Δ2-oxazoline and an anionic ring-opening polymerization of γ-benzyl L-glutamate NCA. The thermo- and pH-responsive aggregation behavior of the polymer in aqueous solution is under investigation.