反应详情

温度

70 °C

A suspension of 5-(3-bromo-4-cyclohexyloxy-phenyl)-6-butyl-pyridazin-3-ol (4.18 mmol, 1.7 g) in POCl3 (20 mL) was kept stirring at 70° C. for 2 h. The reaction mixture was concentrated, to the residue water was added, extracted with ethyl acetate washed with sat NaHCO3 solution, water, brine, dried and concentrated under reduced pressure. The resultant residue was purified by silica gel flash chromatography using a mixture of hexanes in ethyl acetate (9:1) to provide 4-(3-bromo-4-cyclohexyloxy-phenyl)-3-butyl-6-chloro-pyridazine (1.5 g).

1. concentrationThe reaction mixture was concentrated, to the residue water
2. additionwas added
3. extractionextracted with ethyl acetate
4. washwashed with sat NaHCO3 solution, water, brine
5. customdried
6. concentrationconcentrated under reduced pressure
7. customThe resultant residue was purified by silica gel flash chromatography
8. additiona mixture of hexanes in ethyl acetate (9:1)