反应详情

Lithium hydroxide monohydrate (1.63 g, 39.78 mmol) was added to an ice-cooled suspension of 51b) (5 g, 13.26 mmol) in THF/water (1:1, 50 mL) and the resulting mixture was stirred at room temperature for 16 h. The solvents were removed under reduced pressure and the residue was dissolved in water (20 mL). The aqueous solution was washed with ethyl acetate (2×20 mL), acidified with sodium hydrogen sulfate and extracted with dichloromethane (3×50 mL). The combined organic layers were dried over sodium sulfate and evaporated. White solid. Yield: 4 g (83% of theory)

1. temperaturecooled
2. customThe solvents were removed under reduced pressure
3. dissolutionthe residue was dissolved in water (20 mL)
4. washThe aqueous solution was washed with ethyl acetate (2×20 mL)
5. extractionextracted with dichloromethane (3×50 mL)
6. dry with materialThe combined organic layers were dried over sodium sulfate
7. customevaporated