反应详情

A solution of ethyl 7-n-butylamino-1H-pyrazolo[4,3-b]-pyridine-6-carboxylate (524 mg, 2 mmol) in dry THF (15 ml) was added dropwise to a stirred suspension of lithium aluminium hydride (152 mg, 4 mmol) in THF (15 ml). The mixture was heated under reflux under nitrogen for 90 min then cooled. Ether (30 ml), water (0.15 ml), 10% sodium hydroxide solution (0.15 ml) and water (0.45 ml) were added sequentially, with stirring, and the mixture was filtered, then evaporated in vacuo. The glassy residue (300 mg) was recrystallised from ethyl acetate/ether, to give a white solid, m.p. 86°-95° C.

1. temperatureThe mixture was heated
2. temperatureunder reflux under nitrogen for 90 min
3. temperaturethen cooled
4. filtrationthe mixture was filtered
5. customevaporated in vacuo
6. customThe glassy residue (300 mg) was recrystallised from ethyl acetate/ether
7. customto give a white solid, m.p. 86°-95° C.