反应详情

To the product of Example 4, Step A (0.5 g, 1.4 mmol) in THF (3 mL) and MeOH (1.5 mL) was added 3-fluorobenzaldehyde (0.6 mL, 2.8 mmol) and NaOMe (0.2 g, 0.56 mmol). The reaction was stirred at rt overnight, followed by heating at 50° C. for an additional day. The reaction was diluted with EtOAc and washed with saturated aq NaHCO3, brine, dried (Na2SO4), filtered and concentrated The residue was purified by flash chromatography on silica gel gradient eluted with 0-30% EtOAc in hexane to afford the product.

1. temperatureby heating at 50° C. for an additional day
2. washwashed with saturated aq NaHCO3, brine
3. dry with materialdried (Na2SO4)
4. filtrationfiltered
5. concentrationconcentrated The residue
6. customwas purified by flash chromatography on silica gel gradient
7. washeluted with 0-30% EtOAc in hexane
8. customto afford the product