Formic Acid → 4-Amino-3-bromo-2,5-difluorobenzaldehyde
反応式
[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]参加物
4
反応条件
- 温度
- 80 °C
実験手順
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).
後処理
- 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
出典と根拠
- ORDレコード
- ord-7944c7328a8948838f13833457449723
- 出典データセット
- uspto-grants-2013_02
- 特許番号
- US08378104B2
反応ノート
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