反应详情

温度

120 °C

A mixture of 3-(4-benzyloxy-phenyl)-2-hydroxy-4-oxo-octanoic acid ethyl ester (28.08 mmol, 10.8 g) and hydrazine hydrate (15 mL) in acetic acid (45 mL) was stirred at 120° C. for 4 h. The reaction mixture was concentrated under reduced pressure and to the residue was added water (200 mL). This was extracted with DCM (3×200 mL), and the combined organic layer was dried and concentrated under reduced pressure. The resultant residue was purified by flash silica gel column chromatography eluting with 50% ethyl acetate in hexanes to afford 5-(4-benzyloxy-phenyl)-6-butyl-2H-pyridazin-3-one.

1. concentrationThe reaction mixture was concentrated under reduced pressure and to the residue
2. additionwas added water (200 mL)
3. extractionThis was extracted with DCM (3×200 mL)
4. customthe combined organic layer was dried
5. concentrationconcentrated under reduced pressure
6. customThe resultant residue was purified by flash silica gel column chromatography
7. washeluting with 50% ethyl acetate in hexanes