Sodium Azide → 2-Azido-1-(3-(trifluoromethoxy)phenyl)ethanone
반응식
[N-:1]=[N+:2]=[N-:3].[Na+].[F:5][C:6]([F:19])([F:18])[O:7][C:8]1[CH:9]=[C:10]([CH:15]=[CH:16][CH:17]=1)[C:11](=[O:14])[CH2:12]Br>CO>[N:1]([CH2:12][C:11]([C:10]1[CH:15]=[CH:16][CH:17]=[C:8]([O:7][C:6]([F:5])([F:18])[F:19])[CH:9]=1)=[O:14])=[N+:2]=[N-:3]참가 물질
4
실험 절차
Add sodium azide (583 mg, 8.96 mmol) to a solution of 3-(trifluoromethoxy)-phenacyl bromide (2.17 g, 7.66 mmol) in methanol (20 mL). Stir at room temperature for 2 h. Concentrate the mixture in vacuo. Dissolve the residue in EtOAc (20 mL) and wash with water (10 mL). Dry the organic layer (Na2SO4), filter, and concentrate filtrate in vacuo to provide 2-azido-1-(3-(trifluoromethoxy)phenyl)ethanone (1.70 g, 91%). 1H-NMR (CDCl3): δ7.83 (m, 1H), 7.77 (s, 1H), 7.56 (m, 1H), 7.49 (m, 1H), 4.55 (s, 2H).
후처리
- concentrationConcentrate the mixture in vacuo
- dissolutionDissolve the residue in EtOAc (20 mL)
- washwash with water (10 mL)
- dry with materialDry the organic layer (Na2SO4)
- filtrationfilter
- concentrationconcentrate filtrate in vacuo
출처 및 근거
- ORD 기록
- ord-1b0490bc144345f1bf0475e7eaa6ff82
- 출처 데이터셋
- uspto-grants-2012_01
- 특허 번호
- US08093383B2
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