Sodium Azide → 1-(4-Bromophenyl)-1,2-dihydro-5H-tetrazol-5-one
反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]=[C:9]=[O:10])=[CH:4][CH:3]=1.[N-:11]=[N+:12]=[N-:13].[Na+].[Al+3].[Cl-].[Cl-].[Cl-]>C1COCC1>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:9](=[O:10])[NH:13][N:12]=[N:11]2)=[CH:4][CH:3]=1参加物
5
実験手順
To a solution of 1-bromo-4-isocyanatobenzene (5.0 g, 25 mmol) and sodium azide (5.0 g, 77 mmol) in THF (30 mL) was added a solution of AlCl3 (4.0 g, 30 mmol) in THF (18 mL) dropwise. The reaction mixture was heated to reflux overnight. The organic solvent was removed under reduced pressure, then water (50 mL) was added. The solids formed were collected by filtration to obtain compound 53a as a white solid. Mass Spectrum (LCMS, ESI pos.): Calcd. for C7H5BrN4O: 241.0 (M+H). Found 241.1.
後処理
- temperatureThe reaction mixture was heated
- temperatureto reflux overnight
- customThe organic solvent was removed under reduced pressure
- additionwater (50 mL) was added
- customThe solids formed
- filtrationwere collected by filtration
出典と根拠
- ORDレコード
- ord-7df18866f5e34c23955575366b59a661
- 出典データセット
- uspto-grants-2015_11
- 特許番号
- US09193736B2
反応ノート
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