A mixture of a glycosyl acceptor [0.16 mmol] and a glycosyl donor [0.16 mmol, 1 eq.] was co-evaporated with toluene twice and dried for 1 h in vacuo, and then the flask was filled with Ar. Freshly activated molecular sieves 4 Å [100 mg] and anhydrous DCM [2 mL] were added and the mixture was stirred for 2 h at rt. Then, the solution of TMSOTf in DCM [10% v/v, 60 μL, 0.2 eq.] was added at −50 °C under argon protection. The mixture was stirred under argon protection until TLC showed full consumption of the starting materials, and then neutralized with Et3N and the mixture was purified by chromatography (silica gel, eluent: hexane/EtOAc) to give a glycosylation product as a mixture of α- and β-isomers.
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