反应详情

To a solution of 3-acetyl-5-bromopyridine (0.20 g, 1.0 mmol) in tetrahydrofuran (3.3 mL) were added a solution of trimethyl(trifluoromethyl)silane in tetrahydrofuran (0.5 M, 4.0 mL, 2.0 mmol) and a solution of tetrabutylammonium fluoride in tetrahydrofuran (1.0 M, 0.1 mL, 0.1 mmol). The resulting reaction mixture was stirred at room temperature for 1 h, then diluted with water and dichloromethane. The organic layer was separated, dried over magnesium sulfate, filtered and concentrated. Purification by flash chromatography on silica gel (0 to 6% dichloromethane in acetone) provided the title compound: LCMS m/z 271.75 [M+H]+; 1H NMR (500 MHz, CDCl3) δ 8.71 (s, 1 H), 8.68 (s, 1 H), 8.11 (s, 1 H), 3.12 (br s, 1 H), 1.82 (s, 3H).

1. customThe resulting reaction mixture
2. customThe organic layer was separated
3. dry with materialdried over magnesium sulfate
4. filtrationfiltered
5. concentrationconcentrated
6. customPurification by flash chromatography on silica gel (0 to 6% dichloromethane in acetone)