Aldehydes compounds selective converted to 1,1-diacetates as protective reagent with SiO2@FeSO4 nano composite as effective nano catalyst at room temperature under solvent-free condition and acetic anhydride (Ac2O) as acetylation reagent. This method provides several advantages, such as low cost of the nano catalyst, high yields, short reaction time, chemoselective protection of aldehydes and operational simplicity. Aromatic and aliphatic, simple and conjugated aldehydes were protected with excellent yields. In addition, chemoselective reductive acetylation of aldehydes over ketones was achieved perfectly with the reagent at room temperature.Scheme 1. Synthesis of 1,1-diacetates from aldehydes.