反应详情

A 4N solution of hydrochloric acid in ethyl acetate (120 ml) was cooled in an ice bath. tert-Butyl[4-(4-benzyloxycarbonylamino-3-fluorophenoxy)pyridin-2-yl]carbamate (3.92 g) was added thereto while stirring, followed by stirring in an ice bath for 10 min. The reaction mixture was then stirred at room temperature for 3.5 hr. The reaction mixture was concentrated under reduced pressure. Ethyl acetate (150 ml) and a saturated aqueous solution of sodium hydrogencarbonate (70 ml) were added thereto, and liquid-liquid separation was carried out. The aqueous layer was extracted with ethyl acetate (50 ml). The combined organic layer was washed with brine and dried over anhydrous sodium sulfate. The organic layer after drying was concentrated under reduced pressure. The resultant crystals were suspended in a mixed solvent of hexane-ethyl acetate (5:1). The crystals were collected by filtration and washed with a mixed solvent of hexane-ethyl acetate (5:1). The crystals were sucked to dryness at room temperature to provide the titled compound as pale yellow crystals (2.93 g, 95.9%).

1. stirringby stirring in an ice bath for 10 min
2. stirringThe reaction mixture was then stirred at room temperature for 3.5 hr
3. concentrationThe reaction mixture was concentrated under reduced pressure
4. additionEthyl acetate (150 ml) and a saturated aqueous solution of sodium hydrogencarbonate (70 ml) were added
5. customliquid-liquid separation
6. extractionThe aqueous layer was extracted with ethyl acetate (50 ml)
7. washThe combined organic layer was washed with brine
8. dry with materialdried over anhydrous sodium sulfate
9. customThe organic layer after drying
10. concentrationwas concentrated under reduced pressure
11. filtrationThe crystals were collected by filtration
12. washwashed with a mixed solvent of hexane-ethyl acetate (5:1)
13. customwere sucked to dryness at room temperature