反应详情

To a solution of 4-(6-chloro-pyridazin-3-yl)-benzonitrile (20 g, 92.8 mmol) in 1-butanol (150 mL) was added 1-isopropyl-piperazine hydrochloride (29.8 g, 148.5 mmol) and NH4Cl (4.96 g, 92.8 mmol). The reaction mixture was heated at reflux for 48 h and then concentrated under reduced pressure. The residue was dissolved into a 10% solution of citric acid in water and filtered. Solid K2CO3 was added to the filtrate until pH 9. The precipitate was isolated and washed with water to give 4-[6-(4-isopropyl-piperazin-1-yl)-pyridazin-3-yl]-benzonitrile (20 g, 70%).

1. temperatureThe reaction mixture was heated
2. temperatureat reflux for 48 h
3. concentrationconcentrated under reduced pressure
4. dissolutionThe residue was dissolved into a 10% solution of citric acid in water
5. filtrationfiltered
6. additionSolid K2CO3 was added to the filtrate until pH 9
7. customThe precipitate was isolated
8. washwashed with water