反应详情

Crude 5b (23.6 g, 96 mmol) is added during 30 min to a stirred suspension of sodium butanoate (10.5 g, 96 mmol) in dry DMF (125 mL) at -20° C. followed by stirring overnight at ambient temperature. After filtration and washing with DMF (5 mL) and Et2O (10 mL),Et2O (250 mL) and ice-cold H2O (100 mL) are added to the combined filtrates. The aqueous phase is separated and extracted with Et2O (100 mL). The combined organic phases are washed (all solutions ice-cold) with 5% aqueous NaHCO3 (50 mL), H2O (50 mL), 0.01N HCl (100 mL), and H2O (2×50 mL). After drying (MgSO4) and evaporation of solvents the residue is distilled to yield 15.0 g (76%) of 6db, bp 75°-80° C./0.5 mbar.

1. filtrationAfter filtration
2. washwashing with DMF (5 mL) and Et2O (10 mL),Et2O (250 mL) and ice-cold H2O (100 mL)
3. additionare added to the combined filtrates
4. customThe aqueous phase is separated
5. extractionextracted with Et2O (100 mL)
6. washThe combined organic phases are washed (all solutions ice-cold) with 5% aqueous NaHCO3 (50 mL), H2O (50 mL), 0.01N HCl (100 mL), and H2O (2×50 mL)
7. customAfter drying
8. custom(MgSO4) and evaporation of solvents the residue
9. distillationis distilled