Azido(trimethyl)stannane → 5-(2-Bromo-4-chloro-6-fluoro-phenyl)-2H-tetrazole
반응식
[Br:1][C:2]1[CH:9]=[C:8]([Cl:10])[CH:7]=[C:6]([F:11])[C:3]=1[C:4]#[N:5].[N:12]([Sn](C)(C)C)=[N+:13]=[N-:14]>C1(C)C=CC=CC=1>[Br:1][C:2]1[CH:9]=[C:8]([Cl:10])[CH:7]=[C:6]([F:11])[C:3]=1[C:4]1[N:12]=[N:13][NH:14][N:5]=1참가 물질
4
반응 조건
- 온도
- 120 °C
실험 절차
A mixture of 2-bromo-4-chloro-6-fluoro-benzonitrile (4 g, 17.06 mmol) and azidotrimethyltin (3.86 g, 18.77 mmol) in toluene (100 ml) was heated to 120° C. for 72 h. After completion of the reaction, the mixture was partitioned between EtOAc (50 ml) and aqueous 0.5N HCl solution (40 ml). The organic layer was separated, washed with water and brine, dried with Na2SO4 and concentrated under reduced pressure to afford the title compound as red solid (4.2 g, 87%).
후처리
- customAfter completion of the reaction
- customthe mixture was partitioned between EtOAc (50 ml) and aqueous 0.5N HCl solution (40 ml)
- customThe organic layer was separated
- washwashed with water and brine
- dry with materialdried with Na2SO4
- concentrationconcentrated under reduced pressure
출처 및 근거
- ORD 기록
- ord-2a3ec3bb36e24fa59a05eea5a623bc11
- 출처 데이터셋
- uspto-grants-2014_12
- 특허 번호
- US08912221B2
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