반응 #1268693

ord-023f735e6bf5416ca0f2f4f3a198eb17

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONThis solution was then added to a 2 L Parr flask
  2. 2
    workup.ADDITIONcontaining
  3. 3
    기타had been flushed with nitrogen for 15 minutes
  4. 4
    여과The reaction mixture was filtered through a pad of Celite
  5. 5
    세척the Celite washed with ethanol
  6. 6
    농축The filtrate was then concentrated in vacuo

실험 절차

A solution of 1-benzyl-4-(N-tert-butoxycarbonyl-N-isopropylamino)piperidine (79.0 g, 0.24 mol) in ethanol (140 mL) was flushed with nitrogen for 15 minutes. This solution was then added to a 2 L Parr flask containing a mixture of 10% palladium on carbon (15.8 g; ca. 50% wt. water) in ethanol (100 mL), which solution had been flushed with nitrogen for 15 minutes. This reaction mixture was placed on a Parr Shaker under hydrogen at 50 psi for 24 hours. The reaction mixture was filtered through a pad of Celite and the Celite washed with ethanol. The filtrate was then concentrated in vacuo to afford 57.0 g of the title intermediate as a white solid (>99% yield).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07285564B2uspto-grants-2007_10