反应详情

温度

60 °C

A mixture of Example 117A (3.18 g, 15.0 mmol), solid potassium hydroxide (8.4 g, 150 mmol), and a mixture of ethanol (75 mL) and water (15 mL) was heated at about 60° C. overnight. After cooling, the pH of the mixture was adjusted to about 1 by addition of 1N aqueous hydrochloric acid. The mixture was extracted with ethyl acetate (4×50 mL). The combined organic extracts were dried over sodium sulfate, filtered, and concentrated by rotary evaporator to give a tan powder. The crude product was recrystallized from ethyl acetate/hexanes to give the title compound as a white solid that was used without further purification for the next step.

1. temperatureAfter cooling
2. extractionThe mixture was extracted with ethyl acetate (4×50 mL)
3. dry with materialThe combined organic extracts were dried over sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated by rotary evaporator
6. customto give a tan powder
7. customThe crude product was recrystallized from ethyl acetate/hexanes