Formic Acid → 4-Amino-3-bromo-2,5-difluorobenzaldehyde
반응식
[NH2:1][C:2]1[C:9]([F:10])=[CH:8][C:5]([C:6]#N)=[C:4]([F:11])[C:3]=1[Br:12].C(O)=[O:14]>[Ni]>[NH2:1][C:2]1[C:9]([F:10])=[CH:8][C:5]([CH:6]=[O:14])=[C:4]([F:11])[C:3]=1[Br:12]참가 물질
4
반응 조건
- 온도
- 80 °C
실험 절차
To a solution of 4-amino-3-bromo-2,5-difluoro-benzonitrile (7 g, 30 mmol) in 95-97% formic acid (40 mL) was added Raney nickel (7 g, previously washed with water and methanol). The reaction mixture was heated to 75-85° C. for 2 h. The reaction was then cooled to room temperature and filtered through Celite, washing with dichloromethane and water. The dichloromethane layer was washed with aqueous sodium bicarbonate and brine, dried over sodium sulfate, filtered, and concentrated to afford 5 g (71%) of the title compound. 1H NMR (300 MHz, CDCl3): δ 10.15 (s, 1H), 7.41-7.49 (m, 1H), 4.9 (br. s, 2H).
후처리
- washpreviously washed with water and methanol)
- temperatureThe reaction was then cooled to room temperature
- filtrationfiltered through Celite
- washwashing with dichloromethane and water
- washThe dichloromethane layer was washed with aqueous sodium bicarbonate and brine
- dry with materialdried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-7944c7328a8948838f13833457449723
- 출처 데이터셋
- uspto-grants-2013_02
- 특허 번호
- US08378104B2
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