反应详情

温度

75 °C

A solution of ethyl 4-[(8-fluoro-6-methylphenanthridin-5(6H)-yl)sulfonyl]phenyl carbonate (0.45 g, 1.02 mmol) in methanol (5.0 mL) was treated with a 1 N sodium hydroxide (5.1 mL) solution, and heated at 75° C. for 14 hours. After cooling to room temperature, the methanol was evaporated in vacuo. The resulting aqueous mixture was acidified with a 1 N hydrochloric acid solution, diluted with a saturated, aqueous, sodium chloride solution (100 mL), and extracted with dichloromethane (5×15 mL). The combined organic phase was dried over anhydrous sodium sulfate, filtered, and concentrated in vacuo to a white solid. The solid was purified by filtration through a short column of silica gel, eluting with ethyl acetate, to yield the title compound as a homogeneous, white, crystalline, solid (0.34 g, 89%), m.p. 188° C.; MS [(−ESI), m/z]: 368 [M−H]−;

1. temperatureAfter cooling to room temperature
2. customthe methanol was evaporated in vacuo
3. additiondiluted with a saturated, aqueous, sodium chloride solution (100 mL)
4. extractionextracted with dichloromethane (5×15 mL)
5. dry with materialThe combined organic phase was dried over anhydrous sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated in vacuo to a white solid
8. filtrationThe solid was purified by filtration through a short column of silica gel
9. washeluting with ethyl acetate