反应详情

温度

45 °C

Compound 9.7 (3.1 g, 11.8 mmol) in pyridine (15 mL) was treated with benzoyl chloride (4.0 mL, 35 mmol) dropwise and the mixture was stirred at 45° C. for 1 h (significant exotherm upon BzCl addition). The mixture was cooled to 0° C. and EtOH (2 mL) was added dropwise and stirred for 10 minutes. The solution was concentrated in vacuo and the residue was dissolved in EtOAc (100 mL) and washed with 1 N HCl (10 mL) and brine (10 mL). The solution was dried over MgSO4, filtered, and concentrated in vacuo. The residue was treated to silica gel column chromatography (SiO2, 4×20 cm, 50-100% EtOAc-hexanes gradient) to afford compound 9.8 (4.2 g, 75% yield).

1. temperatureThe mixture was cooled to 0° C.
2. stirringstirred for 10 minutes
3. concentrationThe solution was concentrated in vacuo
4. dissolutionthe residue was dissolved in EtOAc (100 mL)
5. washwashed with 1 N HCl (10 mL) and brine (10 mL)
6. dry with materialThe solution was dried over MgSO4
7. filtrationfiltered
8. concentrationconcentrated in vacuo
9. additionThe residue was treated to silica gel column chromatography (SiO2, 4×20 cm, 50-100% EtOAc-hexanes gradient)