反应详情

LiOH (10 mg, 0.42 mmol) in water (0.2 mL) was added to III (25 mg, 0.085 mmol) in THF (0.8 mL) at rt. After 19 h, the reaction mixture was neutralized with 2N HCl, poured onto brine (2 mL), and EtOAc (3 mL) was 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, and then evaporated under reduced pressure. The resulting residue was then purified by silica gel column chromatography using CH2Cl2/MeOH (100:2 to 100:4) as eluant to furnish IV as a colourless oil (11.3 mg, 46%).

1. additionwas added
2. customThe phases were separated
3. extractionthe aqueous phase was extracted with EtOAc (2×3 mL)
4. dry with materialdried over MgSO4
5. filtrationfiltered
6. customevaporated under reduced pressure
7. customThe resulting residue was then purified by silica gel column chromatography