反应详情

To a stirred solution of (R)-tert-butyl 1-benzylpiperidin-3-ylcarbamate (300 mg, 1.03 mmol) in THF (5 mL) at −30° C., LiAlH4 (0.77 mL of 2 M solution in THF, 1.5 mmol) was added dropwise under inert atmosphere. After addition the reaction mixture was warmed to rt and then heated to reflux for 2 h. After completion of the reaction, a 20% aq. solution of NaOH solution (5 mL) was added dropwise to the reaction mixture. The reaction mixture was diluted with EtOAc (50 mL) and the suspension was filtered over a short pad of celite. The filtrate was dried over Na2SO4 and concentrated in vacuo to give the titled intermediate (200 mg, 94%). The compound was used in the further steps without purification. LC-MS: m/z [M+1]=205.

1. additionAfter addition the reaction mixture
2. temperatureheated
3. temperatureto reflux for 2 h
4. customAfter completion of the reaction
5. filtrationthe suspension was filtered over a short pad of celite
6. dry with materialThe filtrate was dried over Na2SO4
7. concentrationconcentrated in vacuo