2-Bromo-5-fluorotoluene → 1-Bromo-4-fluoro-2-methyl-5-nitrobenzene
반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[CH:4][C:3]=1[CH3:9].F[B-](F)(F)F.[O:15]=[N+:16]=[O:17]>ClCCl>[Br:1][C:2]1[CH:7]=[C:6]([N+:16]([O-:17])=[O:15])[C:5]([F:8])=[CH:4][C:3]=1[CH3:9]참가 물질
4
실험 절차
To a stirred solution of 1-bromo-4-fluoro-2-methyl-benzene (15.0 g, 79.8 mmol) in dichloromethane (300 mL) was added nitronium tetrafluoroborate (11.7 g, 87.8 mmol) in portions at 0° C. The mixture was heated at reflux for 5 h and was then poured into ice water. The organic layer was separated and the aqueous phase was extracted with dichloromethane (100 mL×3). The combined organic layers were dried over anhydrous Na2SO4 and evaporated under reduced pressure to give crude 1-bromo-4-fluoro-2-methyl-5-nitrobenzene (18.0 g), which was used directly in the next step.
후처리
- temperatureThe mixture was heated
- temperatureat reflux for 5 h
- customThe organic layer was separated
- extractionthe aqueous phase was extracted with dichloromethane (100 mL×3)
- dry with materialThe combined organic layers were dried over anhydrous Na2SO4
- customevaporated under reduced pressure
출처 및 근거
- ORD 기록
- ord-5f407a25c01940e38dcf5cc645b3817a
- 출처 데이터셋
- uspto-grants-2013_09
- 특허 번호
- US08524767B2
반응 노트
불러오는 중…