Nitric Acid → 2,5-Dibromo-3-nitrothiophene
反応式
[Br:1][C:2]1[S:3][C:4]([Br:7])=[CH:5][CH:6]=1.[N+:8]([O-])([OH:10])=[O:9].S(=O)(=O)(O)O>>[Br:1][C:2]1[S:3][C:4]([Br:7])=[CH:5][C:6]=1[N+:8]([O-:10])=[O:9]参加物
4
反応条件
- 温度
- 0 °C
実験手順
2,5-dibromothiophene (10.0 g, 0.0413 mol) was added in portions to nitric acid (38 mL) and concentrated sulfuric acid (75 mL) cooled at 0° C. with an ice bath. On complete addition, the reaction was removed from the cold bath and was stirred for 30 minutes before the reaction mixture was poured onto ice water (400 mL) and extracted with ethyl acetate. The organic layer was separated, dried (Na2SO4), concentrated under vacuum and the residue purified by silica gel chromatography to afford the title product as solid (1.6 g, 13.7% yield).
後処理
- additionOn complete addition
- customthe reaction was removed from the cold bath
- additionwas poured onto ice water (400 mL)
- extractionextracted with ethyl acetate
- customThe organic layer was separated
- dry with materialdried (Na2SO4)
- concentrationconcentrated under vacuum
- customthe residue purified by silica gel chromatography
出典と根拠
- ORDレコード
- ord-e6ac573c54ac4040b6d6234e05cf553d
- 出典データセット
- uspto-grants-2014_03
- 特許番号
- US08680139B2
反応ノート
読み込み中…