반응 #49201

ord-d6f0973ee99c481db33cdbf78f0d4665

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타purged with argon
  2. 2
    workup.ADDITIONTo the solution was added 10% palladium on carbon (0.825 g)
  3. 3
    기타The flask was purged with hydrogen 2 times
  4. 4
    여과The reaction mixture was filtered through a pad of Celite
  5. 5
    세척washed with methanol
  6. 6
    농축The combined organic layer was concentrated under reduced pressure

실험 절차

Compound 75 (8.25 g, 14.9 mmol) was dissolved in methanol (20 mL) and purged with argon. To the solution was added 10% palladium on carbon (0.825 g). The flask was purged with hydrogen 2 times and stirred further at room temperature under hydrogen atmosphere for 3 h. The disappearance of the starting material was confirmed by the TLC. The reaction mixture was filtered through a pad of Celite and washed with methanol. The combined organic layer was concentrated under reduced pressure to afford amine 76 (6.12 g, 98%) as white solid. This was used as such for the next step.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07745608B2uspto-grants-2010_06