反应详情

温度

0 °C

To a 1 L 4-neck round bottom flask was added LAH (9.42 g, 248 mmol) in dry THF (1000 mL) and the reaction mixture was cooled to 0° C. A solution of methyl 4-amino-1-benzylpiperidine-4-carboxylate (47.0 g, 165 mmol) in dry THF (250 ml) was added and the reaction mixture was allowed to warm to room temperature. The reaction mixture was cooled to 0° C. and quenched with water and filtered. The solid was washed with 50 ml of ethyl acetate. The organic layer of the filtrate was separated, washed with 2×200 ml portions of water and 200 ml of brine, dried over anhydrous sodium sulfate, filtered, and concentrated under reduced pressure to afford the title compound.

1. temperatureto warm to room temperature
2. temperatureThe reaction mixture was cooled to 0° C.
3. customquenched with water
4. filtrationfiltered
5. washThe solid was washed with 50 ml of ethyl acetate
6. customThe organic layer of the filtrate was separated
7. washwashed with 2×200 ml portions of water and 200 ml of brine
8. dry with materialdried over anhydrous sodium sulfate
9. filtrationfiltered
10. concentrationconcentrated under reduced pressure