反应详情

温度

25 °C

To a stirred solution of Compound 16 (1.71 g, 8.0 mmol) and Et3N (2.23 mL, 16 mmol) in EtOH (16 mL) was added a solution of benzoylchloride oxime (1.62 g, 10.4 mmol) in EtOH (16 mL) over 90 min. The solution was stirred at 25° C. for 90 min. Then, the solution was heated to reflux for 24 h. The solution was cooled to 25° C. and concentrated. The crude material was taken up in CH2Cl2 (50 mL) and poured into saturated aqueous NaHCO3 (50 mL), extracted with CH2Cl2 (3×50 mL), dried (Na2SO4), and filtered. Flash chromatography (SiO2, 20% EtOAc-hexanes) provided the title compound (1.32 g, 4.19 mmol, 52%).

1. temperatureThen, the solution was heated
2. temperatureto reflux for 24 h
3. temperatureThe solution was cooled to 25° C.
4. concentrationconcentrated
5. additionpoured into saturated aqueous NaHCO3 (50 mL)
6. extractionextracted with CH2Cl2 (3×50 mL)
7. dry with materialdried (Na2SO4)
8. filtrationfiltered