反应详情

A solution of (R)-benzyl 3-(tert-butoxycarbonyl(methyl)amino)piperidine-1-carboxylate (4.00 g, 11.5 mmol) in methanol (10 mL) was slowly added to a suspension of 5% Pd on activated carbon (2.44 g, 1.15 mmol) in EtOH (20 mL). The reaction mixture was evacuated and back filled with N2 (3 cycles). The reaction vessel was then evacuated and back filled with H2 (3 cycles) using a H2 balloon. The mixture was stirred under H2 atmosphere for 1 hour and filtered through a pad of celite, washing with additional 10% MeOH/EtOAc (3×20 mL). The filtrate collected was concentrated in vacuo to provide (R)-tert-butyl methyl(piperidin-3-yl)carbamate (2.01 g, 82% yield) as an oil. LCMS (APCI+) m/z 215 (M+H)+.

1. customThe reaction mixture was evacuated
2. additionback filled with N2 (3 cycles)
3. customThe reaction vessel was then evacuated
4. additionback filled with H2 (3 cycles)
5. filtrationfiltered through a pad of celite
6. washwashing with additional 10% MeOH/EtOAc (3×20 mL)
7. customThe filtrate collected
8. concentrationwas concentrated in vacuo