反应详情

温度

65 °C

To a mixture of 3-fluorophenanthridin-6-ol (Example 1a, 1.58 g, 7.41 mmol) in phosphorus oxychloride (11.7 g, 7.1 mL, 76 mmol) was added dimethylformamide (0.34 g, 0.46 mmol), and the reaction mixture was warmed to 65° C. and stirred under nitrogen for 1 h. The reaction mixture was cooled to room temperature, followed by the careful addition of ice to the reaction mixture. The mixture was stirred for 20 min, and the extracted with ethyl acetate. The resulting organic layer was washed with saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate, filtered, and evaporated to provide the title compound (1.2 g, 70% yield), which was used without further purification.

1. temperatureThe reaction mixture was cooled to room temperature
2. additionfollowed by the careful addition of ice to the reaction mixture
3. stirringThe mixture was stirred for 20 min
4. extractionthe extracted with ethyl acetate
5. washThe resulting organic layer was washed with saturated aqueous sodium chloride solution
6. dry with materialdried over anhydrous magnesium sulfate
7. filtrationfiltered
8. customevaporated