反应详情

温度

70 °C

A suspension of 5-(4-benzyloxy-phenyl)-6-butyl-2H-pyridazin-3-one (5.4 g, 14.73 mmol) in POCl3 (8 mL) was stirred at 70° C. for 2 h. The reaction mixture was concentrated under reduced pressure, and to the residue was added ice (50 g). The mixture was stirred for 1 h. This was extracted with DCM (3×50 mL), the combined organic layer was dried, filtered and concentrated under reduced pressure. The resultant residue was purified by flash silica gel column chromatography eluting with in 10% ethyl acetate in hexanes to provide 4-(4-benzyloxy-phenyl)-3-butyl-6-chloro-pyridazine.

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. additionto the residue was added ice (50 g)
3. stirringThe mixture was stirred for 1 h
4. extractionThis was extracted with DCM (3×50 mL)
5. customthe combined organic layer was dried
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure
8. customThe resultant residue was purified by flash silica gel column chromatography
9. washeluting with in 10% ethyl acetate in hexanes