反应详情

A mixture of ethyl (3,3,4,4,4-pentafluoro-butane-1-sulfonyl)-acetate (J. Fluorine Chem. 1985, 28(4), 425-440) (2.00 g, 6.70 mmol), trifluoro-methanesulfonic acid 2-trifluoromethylsulfanyl-ethyl ester (1.50 g, 5.36 mmol), and potassium carbonate (2.77 g, 5.36 mmol) in 1,2-dimethoxyethane (100 mL) was stirred overnight at room temperature under nitrogen. The reaction mixture was diluted with H2O (200 mL) and extracted with ethyl acetate (2×150 mL). The combined organic extracts were washed with brine (200 mL), dried over Na2SO4 and concentrated under reduced pressure. The residue was purified by column chromatography (SiO2, hexanes/CH2Cl2 1:1) to provide compound II-3 (0.28 g, 37%) as a white solid.

1. extractionextracted with ethyl acetate (2×150 mL)
2. washThe combined organic extracts were washed with brine (200 mL)
3. dry with materialdried over Na2SO4
4. concentrationconcentrated under reduced pressure
5. customThe residue was purified by column chromatography (SiO2, hexanes/CH2Cl2 1:1)
6. customto provide compound II-3 (0.28 g, 37%) as a white solid