One-pot syntheses of trisaccharides have been accomplished simply by changing the solvent system between the two subsequent glycosylation reactions and utilizing the difference in glycosylation rate between different solvents. By tuning the reactivity of acceptors and donors and performing the first glycosylation in Et2O (low glycosylation rate) and the second in CH2Cl2/Et2O (higher glycosylation rate), trisaccharides were synthesized in high yields (76-84%). [on SciFinder (R)]