反应详情

温度

0 °C

To a suspension of compound 4A (3.5 g, 16 mmol) in THF (64 mL) at 0° C. under Ar was added pyridine (6.5 mL, 80 mmol), followed by trifluoroacetic anhydride (5.6 mL, 40 mmol) dropwise. After addition, the reaction mixture was stirred at 0° C. for 5 min, then pored into H2O (50 mL), extracted with EtOAc (3×100 mL). The combined EtOAc extracts were washed with brine, dried (Na2SO4), and concentrated under reduced pressure to give a crude product, which was purified by crystallization from MeOH-EtOAc-Hexane to furnish the title compound (2.3 g) as a white solid.

1. additionAfter addition
2. extractionextracted with EtOAc (3×100 mL)
3. washThe combined EtOAc extracts were washed with brine
4. dry with materialdried (Na2SO4)
5. concentrationconcentrated under reduced pressure
6. customto give a crude product, which
7. customwas purified by crystallization from MeOH-EtOAc-Hexane