PS-100 spectrometer, and the samples contained Me4Si as internal standards.(1) (l-Bromo-2,2,2-trifluoroethyl)sulfur Pentafluoride. In a typical reaction a 10-mL stainless-steel Hoke cylinder was charged with 10 mmol of SF5CH=CF2 and 11.5 mmol of Br2 and then placed in a 110 °C oven for 24 h. The cylinder was cooled to room temperature and the volatile material condensed onto Hg contained in a 50-mL Pyrex reactor to remove unreacted Br2. After being shaken for 10 min, the remaining mixture was fractionated by °C trap was empty, and the -80 and -95 °C traps contained impure product. The -196 °C trap contained 1.5 mmol of a material identified as FCH(Br)CF3. The -80 and -95 °C traps were combined, and final purification accomplished by gas chromatography, yielding 6.17 mmol (61.7%) of SF6CH(Br)CF3.
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