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.
as an eluent. The resultant material was added to 80 mL of concentrated H2S04 stirred at 0 °C. The reaction mixture was stirred 1.75 h at 0 °C until a homogenous solution was obtained.Ice was added, and the aqueous phase was extracted with ether. The organic phase was dried and the solvent removed under reduced pressure to give an oil which was subjected to MPLC on silica with 1:99 ether/hexane as an eluent to afford a clear, colorless oil. The oil was treated with 2,4-dinitrophenylhydrazone solution to give 2.71 (18%) of the 2,4-dinitrophenylhydrazone of cyclohexyl ethyl ketone as an orange solid, mp 147-148 °C (lit.32 mp 149-151 °C).
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