反应详情

Cesium carbonate (11.4 g, 34.9 mmol) was added to a solution of 3-methylpyridin-2(1H)-one (3.81 g, 34.9 mmol) and 2,2,2-trifluoroethyl trichloromethanesulfonate (9.81 g, 34.9 mmol) in dichloromethane (80 mL). After 2 h, water was added. The mixture was extracted with ether (3×), and the combined organic extracts were dried over sodium sulfate, filtered and concentrated. Purification by silica gel chromatography (100% dichloromethane 25%→methanol/dichloromethane) gave the title compound (3.73 g). MS192.3 (M+1).

1. extractionThe mixture was extracted with ether (3×)
2. dry with materialthe combined organic extracts were dried over sodium sulfate
3. filtrationfiltered
4. concentrationconcentrated
5. customPurification by silica gel chromatography (100% dichloromethane 25%→methanol/dichloromethane)