反应详情

HONH2 (50% aqueous, 0.3 mL) was added to II (32 mg, 0.1 mmol) in DMF (0.3 mL) and THF (0.3 mL) at 0° C. The reaction mixture was agitated at rt for 17 h. Brine (3 mL) and EtOAc (3 mL) were added, the phases were separated, and the aqueous phase was extracted with EtOAc (2×3 mL). The organic phases were combined, dried over MgSO4, filtered then evaporated under reduced pressure. The residue was purified by silica gel column chromatography with CH2Cl2/MeOH (100:3 to 100:10) to furnish IV as a colourless oil (9.6 mg, 30%).

1. customthe phases were separated
2. extractionthe aqueous phase was extracted with EtOAc (2×3 mL)
3. dry with materialdried over MgSO4
4. filtrationfiltered
5. customthen evaporated under reduced pressure
6. customThe residue was purified by silica gel column chromatography with CH2Cl2/MeOH (100:3 to 100:10)