Multigram Laboratory Scale Synthesis of α‑Trifluoromethoxy Carbonyl Compounds

α-trifluoromethoxy carbonyl compounds are valuable building blocks for the synthesis of various trifluoromethoxylated compounds. The best way to easily obtain them is the direct trifluoromethoxylation with the CF3O– anion, generated in situ from trifluoromethyl triflate. However, the necessary autogenous pressure generated during this reaction constitutes a main drawback for a multigram scale extrapolation. A specific procedure using adapted glassware has allowed a laboratory large-scale production (up to 50 g) of such building blocks with good yields.