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A novel, air and thermally stable, yet highly reactive trifluoromethylthiolating reagent, CF3SO2SCF3 (1), was prepared easily in one step from commercially inexpensive CF3SO2Na and Tf2O. 1 is a highly versatile and atom‐efficient reagent that can generate one equivalent of CF3S+, two equivalents of CF3S−, or a combination of CF3S⋅/CF3⋅ species. Many high‐yielding CF3S reactions of C, O, S, and N‐nucleophiles...
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