Tri-block amphiphilic copolymers with hybrid architectures were synthesized by coupling linear （poly（ethylene） glycol）（PEG） and dendritic second-generation Fréchet-type poly（benzyl ether）（PBE） via the Williamson reaction （Gisotv,et al. Angew Chem,Int Ed Engl,1992,31:1200～1202）.Our experimental study shows that the powerful two-dimensional （）1H- （）13C heteronuclear multiple-quantum correlation （HMQC） and two-dimensional （）1H- （）13C heteronuclear multiple-bond correlation （HMBC） NMR techniques rather than the classical one-dimensional （）1H and （）13C-NMR methods can provide clear evidence to verify the formation of the tri-block copolymers.In our measurements HMQC and HMBC NMR techniques directly detected the signal of ether bonds bridged in-between PBE dendrons and PEG blocks,therefore,the formation of the block copolymers are evidently confirmed in molecular level.This work also provides a general method to exactly confirm the formation of block copolymers.
