反应详情

温度

85 °C

To a solution of Preparation 6 (0.05 g, 0.14 mmol) in acetonitrile (1.50 mL) are added potassium carbonate (0.07 g, 0.56 mmol) and 2,2,2-trifluoroethyl trifluoromethanesulfonate (0.06 g, 0.28 mmol). The reaction mixture is heated at 85° C. for 1 h in a microwave, cooled to room temperature and diluted with water. The mixture is extracted with ethyl acetate and the combined organic extracts are dried over sodium sulfate, filtered, and concentrated. The residue is purified by flash column chromatography over silica gel to obtain 30 mg of the title compound as an off-white solid. MS (m/z) 433 (M+1).

1. temperaturecooled to room temperature
2. extractionThe mixture is extracted with ethyl acetate
3. dry with materialthe combined organic extracts are dried over sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated
6. customThe residue is purified by flash column chromatography over silica gel