반응 #166187

ord-2302825d079e47f0adefdbb94b9c8aa3

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타the atmosphere was evacuated
  2. 2
    workup.ADDITIONback-filled with nitrogen
  3. 3
    기타then re-evacuated
  4. 4
    workup.ADDITIONback-filled with hydrogen
  5. 5
    여과before filtering through a pad of Celite®
  6. 6
    세척then washing with ethyl acetate
  7. 7
    농축The filtrate was concentrated in vacuo

실험 절차

A slurry of palladium on carbon (200 mg, 10% wt.) in IMS was added to a degassed solution of 4-cyclopropyl-2-fluoro-1-nitro-benzene (1.45 g, 8 mmol) in IMS (50 mL), the atmosphere was evacuated and back-filled with nitrogen then re-evacuated and back-filled with hydrogen. The reaction mixture was stirred under 1 atmosphere pressure of hydrogen at room temperature for 24 hours before filtering through a pad of Celite® then washing with ethyl acetate. The filtrate was concentrated in vacuo to give the title compound as a pale purple residue (1.19 g, 98%). 1H NMR (CDCl3, 400 MHz) 6.72-6.63 (3 H, m), 3.56 (2 H, s), 1.83-1.75 (1 H, m), 0.93-0.82 (2 H, m), 0.59-0.54 (2 H, m).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08841462B2uspto-grants-2014_09