反应详情

To a stirred solution, under nitrogen, of 13.0 g of 4-(6-chloro-1H-indazol-3-yl)piperidine-1-carboxylic acid methyl ester in 150 ml of tetrahydrofuran was added, dropwise, 48 ml of a 1M solution of lithium aluminum hydride (0.048 mole) in tetrahydrofuran. The solution was stirred under reflux for 1 hr. The reaction mixture was cooled in an ice-salt bath and water was added slowly. The reaction mixture was filtered, the filter cake washed with tetrahydrofuran and methanol, and the filtrate was concentrated. Recrystallization of the residue from ethanol-water yielded 7.6 g (69%) of product, mp 211°-213° C.

1. temperatureunder reflux for 1 hr
2. temperatureThe reaction mixture was cooled in an ice-salt bath
3. filtrationThe reaction mixture was filtered
4. washthe filter cake washed with tetrahydrofuran and methanol
5. concentrationthe filtrate was concentrated
6. customRecrystallization of the residue from ethanol-water