High resolution, two-dimensional1H-n.m.r. spectroscopy has been used to confirm a proposed primary structure of a glycolipid having an octasaccharide head-group. Pure absorption and relay experiments were found to be particularly useful in establishing connectivities in poorly resolved regions of the spectrum. The spectral assignments, which indicate novel linkages including an internal fucopyranosyl residue as well as terminal xylosyl and 4-O-methylglucopyranosyluronic acid groups, add to a growing data base for structural characterization through n.m.r. spectroscopy. © 1986.
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