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-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-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