Preparation and Characterization of Pentafluoro‐λ6‐sulfanyldifluoromethane and Pentafluoro‐λ6‐sulfanyl‐1,1,2,2‐tetrafluoroethane

The pentafluorosulfanyl‐λ6‐perfluoroalkyl halides SF5CF2I, SF5CF2CF2Br, and SF5CF2CF2I were prepared for use in the syntheses of other SF5‐containing compounds. For example, new, convenient syntheses were developed for the hydro compounds SF5CF2H and SF5CF2CF2H from the reduction of these iodides or bromides with either triethylborane or tributyltin hydride. Herein, more thorough spectroscopic analyses of the hydro compounds are presented, including multinuclear NMR and vibrational spectroscopy, mass spectrometry, and computational chemistry. Unfortunately, under the conditions tried, little to no evidence was obtained for potential SF5(CF2)n‐ (where n=1 or 2) transfer reagents such as SF5(CF2)nSi(CH3)3 or Cu(CF2)nSF5.