反应详情

To a solution of N-[2-[4-(6-fluoro-1 H-indazol-3-yl)-1-piperidinyl]ethyl]phthalimide hydrochloride (Example 183) (3.1 g, 7.91 mmol) in THF (100 ml) was added lithium aluminum hydride (16.6 ml of a 1.0M solution in THF, 16.6 mmol) at room temperature, under nitrogen. The reaction mixture was warmed to reflux for 6.5 hours and cooled to room temperature. The reaction was quenched with water (1.5 ml, dropwise) and the precipitated salts were removed via filtration. The solids were washed with DCM and the combined filtrates concentrated to give 2.5 g of the crude product as a solid. The dimaleate salt was prepared in methanol using 3.5 g (>4.0 e.q.) of maleic acid. The light green precipitate was collected via filtration and washed with methanol. Recrystallization from methanol gave 2.1 g of the desired product as an off-white solid, m.p. 196°-199° C.

1. temperatureThe reaction mixture was warmed
2. temperatureto reflux for 6.5 hours
3. customThe reaction was quenched with water (1.5 ml
4. customdropwise) and the precipitated salts were removed via filtration
5. washThe solids were washed with DCM
6. concentrationthe combined filtrates concentrated
7. customto give 2.5 g of the crude product as a solid
8. filtrationThe light green precipitate was collected via filtration
9. washwashed with methanol
10. customRecrystallization from methanol