反应详情

To a solution of 5-(2-fluoropyridin-3-yl)azepan-2-one (0.15 g, 0.72 mmol) in DMF (2.5 mL) under argon was added sodium hydride (0.021 g, 0.86 mmol). The mixture was stirred at room temperature for 15 min before iodomethane (0.054 mL, 0.86 mmol) was added via syringe. This mixture was stirred for 4 h at room temperature before saturated aqueous ammonium chloride was added. The mixture was extracted with ethyl acetate (2×) and the combined extracts were washed with water (3×), saturated aqueous sodium chloride (1×), dried over anhydrous magnesium sulfate, filtered, and concentrated in vacuo to give 5-(2-fluoropyridin-3-yl)-1-methylazepan-2-one. [M+1]=223.1.

1. additionwas added via syringe
2. additionwas added
3. extractionThe mixture was extracted with ethyl acetate (2×)
4. washthe combined extracts were washed with water (3×), saturated aqueous sodium chloride (1×)
5. dry with materialdried over anhydrous magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated in vacuo