反应详情

Phosphorous oxychloride (0.33mL, 3.5 mmol) was added to dry dimethylformamide (3 mL) at 0° C. for 15 minutes. After cooling to room temperature, N-ethyl-(2-benzoyloxyethyl)aniline (1 g, 3.5 mmol) was added followed by stirring at room temperature for 5 minutes and then at 90° C. for 30 minutes. The dark green solution was then cooled to room temperature and made basic to pH 8 by addition of 1 molar sodium hydroxide solution. Product was extracted into diethyl ether (3×20 mL). The combined ether extracts were washed with water (30 mL), saturated sodium chloride (30 mL), dried over magnesium sulfate and solvent removed under reduced pressure. Product was isolated as a clear yellow oil (0.90 g, 82% yield).

1. waitat 90° C. for 30 minutes
2. temperatureThe dark green solution was then cooled to room temperature
3. extractionProduct was extracted into diethyl ether (3×20 mL)
4. washThe combined ether extracts were washed with water (30 mL), saturated sodium chloride (30 mL)
5. dry with materialdried over magnesium sulfate and solvent
6. customremoved under reduced pressure