反应详情

A mixture of 4-(6-chloro-pyridazin-3-yloxy)-benzoic acid methyl ester (1.0 g, 3.78 mmol) from the previous step and anhydrous potassium acetate (0.526 g, 5.37 mmol) in glacial acetic acid (10 ml) was refluxed for 13 h. The volatiles were evaporated in vacuo and the residue was diluted with dichloromethane (20 ml). The separated solid was collected by filtration, washed with 50% aqueous ethanol (2×5 ml) and water (4×7 ml) and dried to provide 0.7 g (43%) of 4-(6-oxo-1,6-dihydro-pyridazin-3-yloxy)-benzoic acid methyl ester.

1. temperaturewas refluxed for 13 h
2. customThe volatiles were evaporated in vacuo
3. additionthe residue was diluted with dichloromethane (20 ml)
4. filtrationThe separated solid was collected by filtration
5. washwashed with 50% aqueous ethanol (2×5 ml) and water (4×7 ml)
6. customdried