反应详情

To a 0° C. solution of Example 59A (1.0 g, 40 mmol) in dichloromethane (3 mL) was added trifluoroacetic acid (3. mL, 40 mmol). The reaction mixture was stirred at ambient temperature for 3 hours then concentrated under reduced pressure. The residue was diluted with ethyl acetate (100 mL) and washed with saturated aqueous NaHCO3. The layers were separated and the aqueous phase was extracted with ethyl acetate (5×100 mL). The combined organic extracts were dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure to provide the title compound. MS (ESI+) m/z 151 (M+H)+.

1. concentrationthen concentrated under reduced pressure
2. additionThe residue was diluted with ethyl acetate (100 mL)
3. washwashed with saturated aqueous NaHCO3
4. customThe layers were separated
5. extractionthe aqueous phase was extracted with ethyl acetate (5×100 mL)
6. dry with materialThe combined organic extracts were dried over anhydrous Na2SO4
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure