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A double regioselective deprotection of symmetrical tethered isopropylidenated monosaccharides has been elaborated. This mild and simple methodology involving iodine and acetonitrile, allows breaking of dioxolane and dioxane moieties and affords new chiral structures in good yields. Spectroscopic characterization of these molecules includes FTIR, ESI-MS, 1 H and 13 C NMR, and also 2D-COSY, HMQC and HMBC measurements.

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