Abstract: Provided are methods for the preparation of glycosylation products, including those represented by formula I: Sugar-O—R???I comprising the step of combining R?—OH, a glycosyl sulfide glycosyl donor (“thioglycoside donor”), a hypervalent iodine alkyl-transfer activating reagent, and a base. In an embodiment, the hypervalent iodine alkyl-transfer activating reagent is (phenyl(trifluoroethyl)iodonium triflimide).