反应详情

温度

0 °C

A solution of methyl 4-(1-(tert-butoxycarbonyl)piperidin-4-yl)nicotinate (2.6 g, 8.1 mmol, 1.0 eq.) in THF (50 mL) was added dropwise to a solution of lithium aluminium hydride (617 mg, 16.3 mmol, 2.0 eq.) in THF (100 mL) at 0° C. under nitrogen. The resulting solution was stirred for 0.5 hours while the temperature was maintained at 0° C. in an ice/salt bath. The reaction was then quenched with water (0.6 mL) and 15% NaOH (1.8 mL). The mixture was stirred for 10 minutes. The solids were filtered and washed with EtOAc (30 mL). The filtrate was dried over anhydrous Na2SO4 and concentrated under vacuum. The residue was applied onto a silica gel column and eluted with EtOAc/MeOH (10:1) to yield the title compound (1.6 g) as a white solid. ES m/z: [M+H]+293.

1. customThe reaction was then quenched with water (0.6 mL) and 15% NaOH (1.8 mL)
2. stirringThe mixture was stirred for 10 minutes
3. filtrationThe solids were filtered
4. washwashed with EtOAc (30 mL)
5. dry with materialThe filtrate was dried over anhydrous Na2SO4
6. concentrationconcentrated under vacuum
7. washeluted with EtOAc/MeOH (10:1)