An efficient method for the synthesis of 1,1-diacetates (acylals) from different aldehydes in the presence of SO2 4 =SnO2 and acetic anhydride under solvent-free conditions at ambient temperature is achieved. Selective conversion of aldehydes was observed in the presence of ketones. The deprotection of acylals has also been achieved using SO2 4 =SnO2 in methanol. SO2 4 =SnO2 catalyst was characterized by XRD, SEM, IR and BET surface area techniques. The catalyst was found to possess good activity and considerable level of reusability.