反应详情

A mixture of 4-chloro-6-methoxyquinoline (0.97 g, 5 mmol), piperazine (4.3 g, 50 mmol) and glacial acetic acid (0.3 ml) was heated under reflux with stirring in dipropyleneglycolmonomethylether for 48 hours. The mixture was filtered, the filtrate was evaporated to dryness under reduced pressure and the raw product was purified by column chromatography on a silica column using ethyl acetate and methanol with the addition of 0.1% NH3 to yield 0.85 g of a brown solid (3.3 mmol, 66%). MS (ES) m/z=243.8 [M+H]+.

1. temperaturewas heated
2. temperatureunder reflux
3. filtrationThe mixture was filtered
4. customthe filtrate was evaporated to dryness under reduced pressure
5. customthe raw product was purified by column chromatography on a silica column
6. additionwith the addition of 0.1% NH3