反应详情

A mixture of 37 g of 6-(3-aminophenyl)-3(2H)-pyridazinone and 500 ml of acetic anhydride was heated at 85°-90° C. for 8 hours. The solvent was removed in vacuo and the residue dissolved in 500 ml of methanol. To this solution was added portionwise 40 g of potassium hydroxide. The solution was refluxed for 3 hours and the solvent removed in vacuo. The residue was dissolved in water and the solution neutralized with hydrochloric acid. The resulting solid was collected and recrystallized from dichloromethane-methanol, giving 10.8 g of the desired compound as crystals, mp 250°-252° C. (dec.).

1. temperaturewas heated at 85°-90° C. for 8 hours
2. customThe solvent was removed in vacuo
3. dissolutionthe residue dissolved in 500 ml of methanol
4. additionTo this solution was added portionwise 40 g of potassium hydroxide
5. temperatureThe solution was refluxed for 3 hours
6. customthe solvent removed in vacuo
7. dissolutionThe residue was dissolved in water
8. customThe resulting solid was collected
9. customrecrystallized from dichloromethane-methanol