New amphiphilic triblock copoly(2-oxazoline) s, containing hydrophobic domains with fluorine-containing blocks, were synthesized. Using microwave radiation as heating source, triblock copolymers with narrow molar mass distributions were obtained by the sequential addition of 2-ethyl-2-oxazoline, 2-(1-ethylheptyl)-2-oxazoline, and 2-(2,6-difluorophenyl)-2-oxazoline. The polymers obtained were characterized by size exclusion chromatography, H-1 NMR spectroscopy and matrix-assisted laser desorption/ ionization time-of-flight mass spectrometry (MALDI-TOF MS). To investigate the incorporation of all three monomers into the triblock copolymers, a model polymer was prepared with shorter blocks exhibiting a suitable length to be measured in the reflector mode of a MALDI-TOF MS. In addition, kinetic investigations on the homopolymerizations of all monomers were performed in nitromethane at 140 degrees C, yielding the polymerization rates under these conditions. DSC measurements of poly(2-(1-ethylheptyl)-2-oxazoline) and poly(2-(2,6-difluorophenyl)-2-oxazoline)) revealing glass transitions at about 33 and 120 degrees C, respectively. The thermal analysis of a blend of the two polymers showed two glass transitions revealing demixing, which could be an indicating for the immiscibility of the two components in the block copolymers. (C) 2010 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 48: 5100-5108, 2010