Hydrochloric Acid → 3-(Difluoromethyl)-4-fluoroaniline
반응식
[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]참가 물질
5
실험 절차
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).
후처리
- customThe reaction mass was quenched in ice-water
- extractionextracted with DCM
- customThe organic layer was dried
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-182eba89c9924177b9238e987a6b84f0
- 출처 데이터셋
- uspto-grants-2015_08
- 특허 번호
- US09096545B2
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