反应详情

4.5 g of potassium nonaflate is suspended in 15 ml of water. To the solution is added 4.93 g of the crude (4-methylphenyl)(4′-isobutylphenyl)iodonium hydrogensulfate dissolved in 10 ml of methanol. The mixture is stirred for 1 hour at room temperature. 15 ml of methylene chloride is added to the solution and stirred overnight at room temperature. The product is extracted with methylene chloride and the organic layer is washed with water, dried over MgSO4, and concentrated. The residue is purified by flash chromatography on silica gel with methylene chloride and ethanol (95:5) as eluent, yielding 2.46 g (3.8 mmol; 34%) of (4-methylphenyl)(4′-isobutylphenyl)iodonium nonaflate as a brown resin. The structure is confirmed by the 1H-NMR spectrum (CDCl3). δ [ppm]: 0.88 (d, 6H), 1.84 (m,1H), 2.41 (s, 3H), 2.50 (d, 2H), 7.21-7.26 (m, 4H), 7.84 (d, 4H). Elemental analysis: calculation for C21H20O3F9SI

1. stirringstirred overnight at room temperature
2. extractionThe product is extracted with methylene chloride
3. washthe organic layer is washed with water
4. dry with materialdried over MgSO4
5. concentrationconcentrated
6. customThe residue is purified by flash chromatography on silica gel with methylene chloride and ethanol (95:5) as eluent