反应详情

Amide 24-3 (1.0 g, 3.4 mmol) was dissolved in 7 mL toluene at 0°, and BH3 ·DMS (341 μL, 3.6 mmol) was added. After 15 min, the reaction was heated to reflux for 16 h, cooled to 0°, and quenched with 10% Na2CO3. The mixture was extracted with EtOAc, the organic phase was washed with water and brine, dried (MgSO4), concentrated, and purified by flash chromatography (silica, 70% EtOAc/hexane) providing 24-4 as a white solid. Rf 0.64 (silica, EtOAc).

1. temperaturethe reaction was heated
2. temperatureto reflux for 16 h
3. temperaturecooled to 0°
4. customquenched with 10% Na2CO3
5. extractionThe mixture was extracted with EtOAc
6. washthe organic phase was washed with water and brine
7. dry with materialdried (MgSO4)
8. concentrationconcentrated
9. custompurified by flash chromatography (silica, 70% EtOAc/hexane)