反应详情

1.2 g (2.9 mmol) of the compound from Example 70, 0.4 g (6 mmol) of hydroxylammonium chloride and 0.48 g (6 mmol) of sodium acetate in 45 ml of H2O/EtOH (2:1) were refluxed for 30 minutes. The organic solvent was removed under reduced pressure, and the resulting aqueous phase was extracted with ethyl acetate. The organic phase was dried and concentrated under reduced pressure. The residue was recrystallized from ethanol to yield 1.6 g (70%) of the product. Melting point >250° C.

1. customThe organic solvent was removed under reduced pressure
2. extractionthe resulting aqueous phase was extracted with ethyl acetate
3. customThe organic phase was dried
4. concentrationconcentrated under reduced pressure
5. customThe residue was recrystallized from ethanol