Abstract
Two new homonuclear three-dimensional NMR techniques are described for the simplification of proton resonance assignment in oligosaccharides, namely HOHAHA-COSY and ROESY-COSY. The former technique is of value in the resonance assignment of gluco-configuration monosac-charide residues, whereas the latter is more suited to resonance assignment of galacto-configuration monosac-charide residues. The value of these techniques is illustrated by application to the proton resonance assignment of the pentasaccharide Galβ1–4(Fucαl–3)GlcNAcβ1–3 Galβ1–4Glc, a compound which exhibits a variety of assignment problems due to severe cross-peak overlap in conventional COSY or HOHAHA spectra.

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