Abstract
Crystalline α- and β-(1(r)2, 1(r)3 and 1(r)4)-linked methyl β-D-xylobiosides have been obtained by procedures based on condensation of 2,3,4-tri-O-acetyl-α-D-xylopyranosyl bromide with positionally isomeric methyl di-O-acetyl-β-D-xylopyranosides, followed by deacetylation. Per-O-acetates of the isomeric methyl β-D-xylobiosides were also obtained crystalline. The β-linked disaccharide methyl glycosides, methylated on a preparative scale, gave crystalline fully methylated products.