Nitric Acid → 2,5-Dibromo-3-nitrothiophene
반응식
[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]참가 물질
4
반응 조건
- 온도
- 0 °C
실험 절차
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).
후처리
- 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
출처 및 근거
- ORD 기록
- ord-e6ac573c54ac4040b6d6234e05cf553d
- 출처 데이터셋
- uspto-grants-2014_03
- 특허 번호
- US08680139B2
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