Sodium Azide → 1-(4-Bromophenyl)-1,2-dihydro-5H-tetrazol-5-one
반응식
[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]=1참가 물질
5
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-7df18866f5e34c23955575366b59a661
- 출처 데이터셋
- uspto-grants-2015_11
- 특허 번호
- US09193736B2
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