Interresidue coupling constants (/sup 3/J/sub C1-C1'/ approx. beta.DGal(1.->.4)DGlcNAc resulted in a similar pattern of chemical shift changes. beta.DGal(1.->.4).beta.DGlcNAc-hexanolamine caused more » a 5.6 ppm downfield shift of the C2 resonance of Gal. Specific /sup 13/C enrichment and comparison with /sup 13/C-enriched model compounds allowed unambiguous assignment of /sup 13/C resonances. The following oligosaccharides were prepared and purified by ion-exchange and gel-filtration chromatography. Partially purified glycosyltransferases and chemically synthesized sugar nucleotides have been used to prepare a number of oligosaccharides related to the type 2 (human) blood group (H) substance.