反应详情

To a 20-mL scintillation vial containing a magnetic stir bar were added the product from Example 104A (143 mg, 0.350 mmol), anhydrous dichloromethane (5 mL), and trifluoroacetic acid (200 mg, 1.75 mmol). The pale yellow solution was stirred at room temperature for 4 hours. The pH of the reaction mixture was adjusted to 9 by addition of saturated aqueous sodium bicarbonate solution. The mixture was extracted with dichloromethane (3×10 mL). The combined organic extracts were dried (MgSO4), filtered, and concentrated by rotary evaporator to afford the title compound. The crude product was used without purification for the next step. MS (ESI+) m/z 310 (M+H)+.

1. additionTo a 20-mL scintillation vial containing a magnetic stir bar
2. extractionThe mixture was extracted with dichloromethane (3×10 mL)
3. dry with materialThe combined organic extracts were dried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrated by rotary evaporator