반응 #89769

ord-84c821dd17b14803a8d591a9a785515d

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과filtered through a pad of Celite
  2. 2
    세척washed with EtOAc
  3. 3
    농축The filtrate was concentrated in vacuo

실험 절차

To a solution of (1S,2S,5S)-5-[(S)-iodo(phenyl)methyl]-2-[4-(4-iodophenyl)piperazin-1-yl]carbonyl-6-oxabicyclo[3.2.1]octan-7-one (49.0 mg, 0.0000747 mol) in ethyl acetate (5.0 mL, 0.051 mol) in a Parr bottle was added Calcium carbonate (15 mg, 0.00015 mol) and palladium (20 mg, 0.00002 mol) (as 10% Pd/C). The reaction mixture was stirred under hydrogen at 55 psi for 18 h. The reaction mixture was diluted with EtOAc, filtered through a pad of Celite and washed with EtOAc. The filtrate was concentrated in vacuo to give the crude product. (30 mg, 100% in yield). MS (ESI): (M+H)+=405.1.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09440958B2uspto-grants-2016_09