反应详情

To a stirred suspension, under nitrogen, of 14.0 g of 3-(1-acetyl-4-piperidinyl)-6-fluoro-1H-indazole in 180 ml of tetrahydrofuran was added, dropwise, 55 ml of a 1M solution of lithium aluminum hydride in tetrahydrofuran. The reaction mixture was stirred under reflux for 1 hr and then stirred at ambient temperature for 15 hrs. The reaction mixture was cooled in an ice-salt bath and water was added slowly. The reaction mixture was filtered. The filter cake was washed with tetrahydrofuran and the filtrate was concentrated. Recrystallization of the residue from toluene afforded 9.0 g (68%) of product. Recrystallization of a 3.0 g sample from toluene yielded the analytical sample, mp 175°-178° C.

1. temperatureunder reflux for 1 hr
2. stirringstirred at ambient temperature for 15 hrs
3. temperatureThe reaction mixture was cooled in an ice-salt bath
4. filtrationThe reaction mixture was filtered
5. washThe filter cake was washed with tetrahydrofuran
6. concentrationthe filtrate was concentrated
7. customRecrystallization of the residue from toluene