反应详情

HONH2 (50% aqueous, 0.3 mL) was added to IV (32 mg, 0.1 mmol) in DMF (0.3 mL) and THF (0.3 mL) at 0° C. The reaction mixture was stirred at rt for 17 h, after which 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 then combined, dried over MgSO4, filtered, and subsequently evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography using CH2Cl2/MeOH (100:3 to 100:10) as eluant to furnish V, 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. customsubsequently evaporated under reduced pressure
6. customThe resulting residue was purified by silica gel column chromatography
7. customto furnish V