反应详情

温度

77.5 °C

To a solution of 97 (330.0 mg; 0.74 mmol) in tetrahydrofuran (8 mL) and methanol (2 mL) was added aqueous lithium hydroxide (4 mL; 2M). The reaction mixture was heated at 75-80° C. for 6 hours, allowed to cool to room temperature and then concentrated under reduced pressure. The resulting residue was dissolved in chloroform (15 mL) and washed with aqueous hydrochloric acid (2×10 mL; 2N). The organic phase was dried over magnesium sulfate, filtered, and concentrated under reduced pressure. The crude residue was purified by preparative HPLC to afford the title compound as a white solid (110 mg).

1. temperatureto cool to room temperature
2. concentrationconcentrated under reduced pressure
3. dissolutionThe resulting residue was dissolved in chloroform (15 mL)
4. washwashed with aqueous hydrochloric acid (2×10 mL; 2N)
5. dry with materialThe organic phase was dried over magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure
8. customThe crude residue was purified by preparative HPLC