反应详情

温度

0 °C

BAL 01028A was prepared in accordance with method D using 3-bromo-4-pyridinecarboxaldehyde (1.010 g, 5.43 mmol), KOH (0.305 g, 5.43 mmol) in methanol (5 mL) and 2-isocyano-1-pyrrolidin-1-yl-ethanone BLE 04134 (0.75 g, 5.43 mmol). The mixture was stirred at 0° C. until precipitation and concentrated. The mixture was partitioned between EtOAc (50 ml) and H2O (25 ml). The aqueous layer was extracted twice with EtOAc (25 mL). The EtOAc fractions were combined, washed twice with brine (2×25 mL), dried over MgSO4 and filtered. After evaporation and trans-(5-(3-bromopyridin-4-yl)-4,5-dihydrooxazol-4-yl)(pyrrolidin-1-yl)methanone BAL 01028A was obtained (1.20 g, 68% yield) as a white solid.

1. customBAL 01028A was prepared in accordance with method D
2. concentrationconcentrated
3. customThe mixture was partitioned between EtOAc (50 ml) and H2O (25 ml)
4. extractionThe aqueous layer was extracted twice with EtOAc (25 mL)
5. washwashed twice with brine (2×25 mL)
6. dry with materialdried over MgSO4
7. filtrationfiltered
8. customAfter evaporation