Hydrochloric Acid → 3-(Difluoromethyl)-4-fluoroaniline
反応式
[F:1][CH:2]([F:13])[C:3]1[CH:8]=[C:7]([N+:9]([O-])=O)[CH:6]=[CH:5][C:4]=1[F:12].Cl>CO.[Fe]>[F:13][CH:2]([F:1])[C:3]1[CH:8]=[C:7]([CH:6]=[CH:5][C:4]=1[F:12])[NH2:9]参加物
5
実験手順
A solution of 2-(difluoromethyl)-1-fluoro-4-nitrobenzene (1.2 g, 6.2 mmol) in methanol (20 mL) was added iron powder (4.8 g, 24.8 mmol) followed by conc. HCl (5 mL) dropwise. The reaction mass was stirred at RT for 1-2 h. The reaction mass was quenched in ice-water, basified with NaHCO3 and extracted with DCM. The organic layer was dried and concentrated to afford 0.800 g of desired product. 1H NMR (300 MHz, DMSO d6): δ 5.25 (s, 2H), 6.66-6.73 (m, 2H), 6.86-7.04 (m, 2H).
後処理
- customThe reaction mass was quenched in ice-water
- extractionextracted with DCM
- customThe organic layer was dried
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-832e639c0de84943ba9acb6ba35acf26
- 出典データセット
- uspto-grants-2016_09
- 特許番号
- US09439890B2
反応ノート
読み込み中…