Alcohols and phenols protection is one of the most broadly used reactions in organic synthesis [1,2] and can be normally obtain by acylation with anhydrides or acyl chlorides in the presence of tertiary amine bases like either pyridine; Lewis or protic acids; or occasionally solid acid catalysts [3,4]. Nano-Fe R 2 R OR R is a powerful catalyst for the acetylation of alcohols. The acetylation of alcohols and phenols carried out with acetic anhydride at 50 ºC in the presence of nano-sized Fe R 2 R OR 3 3 R as catalyst under solvent free conditions in good to excellent yields. The reaction by application of nano-Fe R 2 R OR R afforded the desired ester in high yield. With the increase of various alcohols (1 mmol) and Nano- FeR 3 R (0.01 mmol, 0.03 g) and acetic anhydride (0.02 mmol) proper conditions are created for this reaction to take place. After the completion of the reaction which was monitored by TLC using n-hexane: EtOAc (3:1), and then our products were extracted by thin layer chromatography. The resulting products were determined by their GC spectrums and compared with the authentic samples. 2 R OR 3

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