Ac onvenient methodf or deoxyfluorination of aromatic and aliphatic carboxylic acids with CF 3 SO 2 OCF 3 in the presence of as uitableb ase at room temperature has been developed. The reactiona llows as traightforward access to av ariety of acyl fluorides and provest hat CF 3 SO 2 OCF 3 is an effective deoxyfluorination reagent for carboxylic acids. The method features simplicity,e xpeditiousness, highefficiency,e ase of handling, good functional group tolerance, aw ide range of substrates, excellent yields of products,c ompatibilityo fm any amine initiators, use of environmentally friendly reagents, and effortless removal of byproducts. This reaction represents the first utilization of trifluoromethylt rifluoromethanesulfonatea sa fluorinationr eagent. Scheme1.Synthesis of acyl fluorides from carboxylic acids with different fluorination reagents (selected).