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An example of the use of trimethylsilyl trifluoromethanesulfonate as catalyst is the reaction of β-D-glucopyranoside (1) with acetals (R1 = Me, Ph; R2 = H, CH2Ph, n-C3H7, CH2CH(OMe)2, CH2OMe etc.). It leads highly stereoselectively to the l,l′-diacetals (2) in good yields.