A novel one-pot synthesis of a variety of O-peralkylated δ-aldonolactones 9 from their corresponding glycosides 1 is introduced. This facile procedure involves combining glycoside precursor, tin (IV) chloride and trimethylsilyl azide in methylene chloride at room temperature to furnish the title compounds in moderate to high yields. A side reaction involving extrusion of C-1 of the common carbohydrate intermediate leads to d-arabino- ...