Sodium Azide → 2-Azido-1-(3-(trifluoromethoxy)phenyl)ethanone
反応式
[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]参加物
4
実験手順
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).
後処理
- 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
出典と根拠
- ORDレコード
- ord-1b0490bc144345f1bf0475e7eaa6ff82
- 出典データセット
- uspto-grants-2012_01
- 特許番号
- US08093383B2
反応ノート
読み込み中…