反应详情

温度

80 °C

The chloride, Intermediate 1E (0.97 g, 3.15 mmol) was dissolved in acetonitrile (30 mL) and TEA (1.77 mL, 12.62 mmol) was added drop wise. The resulting mixture was stirred at 80° C. under nitrogen overnight. The mixture was allowed to cool, was filtered and the filtrate was concentrated. The residue was partitioned between DCM and saturated NaHCO3 solution and the phases were separated. The aqueous phase was further extracted with DCM and combined organic extracts were dried over anhydrous MgSO4, filtered and concentrated. The crude residue was purified using normal phase chromatography, eluting with a 0-40% methanol/DCM gradient to provide product Intermediate 1F (0.58 g, 66%) as a brown solid.

1. temperatureto cool
2. filtrationwas filtered
3. concentrationthe filtrate was concentrated
4. customThe residue was partitioned between DCM and saturated NaHCO3 solution
5. customthe phases were separated
6. extractionThe aqueous phase was further extracted with DCM
7. dry with materialwere dried over anhydrous MgSO4
8. filtrationfiltered
9. concentrationconcentrated
10. customThe crude residue was purified
11. washeluting with a 0-40% methanol/DCM gradient