Formic Acid → 4-Bromo-1H-benzimidazole
反応式
[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([NH2:8])[C:3]=1[NH2:9].[CH:10](O)=O>>[Br:1][C:2]1[C:3]2[N:9]=[CH:10][NH:8][C:4]=2[CH:5]=[CH:6][CH:7]=1参加物
3
実験手順
A mixture of 3-bromobenzene-1,2-diamine (1.5 g, 8 mmol) in formic acid (10 mL) was heated at reflux for 2 h. The reaction mixture was concentrated in vacuo. To the residue was added a satd. aq. solution of NaHCO3 and mixture was extracted with EtOAc. The combined extracts was dried (MgSO4), filtered, and evaporated in vacuo to afford 4-bromo-1H-benzo[d]imidazole as a gray solid (1.5 g, 95%). MS (ESI): m/z=197 [M+1]+.
後処理
- temperaturewas heated
- temperatureat reflux for 2 h
- concentrationThe reaction mixture was concentrated in vacuo
- additionTo the residue was added a satd
- extractionaq. solution of NaHCO3 and mixture was extracted with EtOAc
- dry with materialThe combined extracts was dried (MgSO4)
- filtrationfiltered
- customevaporated in vacuo
出典と根拠
- ORDレコード
- ord-77048661ffa64f14b2bd1fd072aa6b18
- 出典データセット
- uspto-grants-2014_01
- 特許番号
- US08637537B2
反応ノート
読み込み中…