반응 #166187
ord-2302825d079e47f0adefdbb94b9c8aa3
반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1기타the atmosphere was evacuated
- 2workup.ADDITIONback-filled with nitrogen
- 3기타then re-evacuated
- 4workup.ADDITIONback-filled with hydrogen
- 5여과before filtering through a pad of Celite®
- 6세척then washing with ethyl acetate
- 7농축The 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).