反应详情

A mixture of 3-[2-(2-oxocyclohexyl)-3-oxo-2,3-dihydropyridazin-6-yl]-2-phenylpyrazolo[1,5-a]pyridine (231 mg), semicarbazide hydrochloride (101 mg), potassium carbonate (125 mg), water (2 ml), and ethanol (10 ml) was heated under reflux for 4 hours. Ethanol was evaporated in vacuo and the residue was partitioned between dichloromethane (30 ml) and saturated aqueous sodium bicarbonate (30 ml). After an additional extraction with dichloromethane, the combined extracts were washed with brine (20 ml), dried over anhydrous sodium sulfate, and evaporated in vacuo to give colorless crystals of 3-[2-(2-carbamoylhydrazonocyclohexyl)-3-oxo-2,3-dihydropyridazin-6-yl]-2-phenylpyrazolo[1,5-a]pyridine (125.8 mg).

1. temperaturewas heated
2. temperatureunder reflux for 4 hours
3. customEthanol was evaporated in vacuo
4. customthe residue was partitioned between dichloromethane (30 ml) and saturated aqueous sodium bicarbonate (30 ml)
5. extractionAfter an additional extraction with dichloromethane
6. washthe combined extracts were washed with brine (20 ml)
7. dry with materialdried over anhydrous sodium sulfate
8. customevaporated in vacuo