반응 #495314

ord-23b4bb9894a143269140182c9a6a5f66

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The mixture was degassed under N2 (3 cycles)
  2. 2
    workup.ADDITIONback filled with H2 (3 cycles)
  3. 3
    여과The reaction mixture was then filtered through a pad of celite
  4. 4
    세척washing with 5% MeOH/EtOAc (3×30 mL)
  5. 5
    기타The filtrate collected
  6. 6
    농축was concentrated in vacuo

실험 절차

A solution of (R)-benzyl 3-(tert-butoxycarbonyl(ethyl)amino)piperidine-1-carboxylate (5.00 g, 13.8 mmol) in a mixture of EtOH:MeOH (1:1, 50 mL) was added to a suspension of 10% palladium on activated carbon (1.47 g, 1.38 mmol) in EtOH (20 mL) under N2 atmosphere. The mixture was degassed under N2 (3 cycles) and back filled with H2 (3 cycles) using a H2 balloon. The mixture was then stirred under H2 atmosphere for 4 hours. The reaction mixture was then filtered through a pad of celite washing with 5% MeOH/EtOAc (3×30 mL). The filtrate collected was concentrated in vacuo to provide the crude (R)-tert-butyl ethyl(piperidin-3-yl)carbamate. LCMS (APCI+) m/z 229 (M+H)+.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08758830B2uspto-grants-2014_06