<i>O</i>-Glycosidation and Knoeings-Knorr procedures were explored.  The synthesis of 6,6^/-diamino-6,6^/-dideoxy-<span style='font-family:Symbol'>a-<span style='font-family:Symbol'>a-trehalose was achieved and derivatives made.  Ester linked tri- and tetra-saccharides were synthesised and the self metathesis of alkyl mono and di-saccharide carried out. The glassy phase of these synthesised oligosaccharide derivatives were investigated for their use as controlled release excipients with two model drugs.  The process of devitrification of these glassy carbohydrate materials was explored.