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Example 3 2Methoxyphenyl trifluoromethyl sulfide A mixture of 6.04 g of bis(2-methoxyphenyl) disulfide, 6.60 g of anhydrous potassium trifluoroacetate, and 9 ml of dry tetramethylene sulfone was stirred in a vacuum distillation apparatus at a pressure of 65 mbar. The mixture was slowly heated in an oil bath up to a maximum of 220 C., during which time volatile products were collected in a receiver that was cooled using dry ice. Redistillation of the crude product gave 3.20 g (70% of theory) of analytically pure 2-methoxyphenyl trifluoromethyl sulfide (boiling point 80 C. at 20 mbar). The 19F NMR data agreed with the data published in J. Org. Chem., 59, 4047 (1985). The structure was additionally confirmed by the 1H NMR and MS spectra.
Example 10 (comparison) By the method of Tetrahedron Lett., 37, 9057 (1996), a mixture of 9.15 g of bis(2-nitrophenyl) disulfide, 9.15 g of anhydrous potassium trifluoroacetate, and 15 ml of dry tetramethylene sulfone was heated to 230 C. with stirring in a distillation apparatus at atmospheric pressure, and volatile products were collected in a receiver which was cooled with dry ice (-78 C.). The crude product was poured into water. Phase separation gave 1.63 g (24.6% of theory) of crude 2-nitrophenyl trifluoromethyl sulfide.