반응 #49172

ord-a58bde882d654e5c9f825f4ce9a5c1f8

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 (2 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 ethyl acetate
  6. 6
    농축The combined organic layer was concentrated under reduced pressure

실험 절차

Compound 4a (14.5 g, 21.7 mmol) was dissolved in ethyl acetate (100 mL) and purged with argon. To the solution was added 10% palladium on carbon (2 g). The flask was purged with hydrogen 2 times and stirred further at room temperature under hydrogen atmosphere for overnight. The disappearance of the starting material was confirmed by the TLC. The reaction mixture was filtered through a pad of Celite and washed with ethyl acetate. The combined organic layer was concentrated under reduced pressure to afford compound 5 (10.56 g, 91%) as white solid. This was used as such for the next step.

출처

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