The microwave-assisted statistical copolymerization of 2-phenyl-2-oxazoline with 2-methyl-2-oxazoline or 2-ethyl-2-oxazoline is discussed in this contribution. Kinetic studies of these statistical copolymerizations as well as reactivity ratio determinations were performed to investigate the monomer distribution in these copoly(2-oxazoline)s, demonstrating the formation of quasi-diblock copolymers. In addition, the synthesis of copolymer series with monomer concentrations ranging from 0 to 100 mol % is described. These copolymer series were characterized with H-1 NMR spectroscopy, gas chromatography, and gel permeation chromatography. Moreover, the glass-transition temperatures and solubility of these copolymers were studied, and this revealing better mixing of poly(2-methyl-2-oxazoline) (pMeOx) with poly(2-phenyl-2-oxazoline) (pPhOx) than poly(2-ethyl-2-oxazoline) (pEtOx) with poly(2-phenyl-2-oxazoline) (pPhOx). (c) 2006 Wiley Periodicals, Inc.