Ammonium Chloride → 2-Amino-4-bromo-5-fluorophenol
반응식
[Br:1][C:2]1[C:7]([F:8])=[CH:6][C:5]([OH:9])=[C:4]([N+:10]([O-])=O)[CH:3]=1.[Cl-].[NH4+]>CO.C1COCC1.[Zn]>[NH2:10][C:4]1[CH:3]=[C:2]([Br:1])[C:7]([F:8])=[CH:6][C:5]=1[OH:9]참가 물질
6
실험 절차
To a solution of 4-bromo-5-fluoro-2-nitrophenol (40.0 g, 169 mmol) in MeOH (250 mL) and THF (250 mL) was added zinc powder (91.0 g, 1700 mmol) and ammonium chloride (111.0 g, 1700 mmol) and the reaction mixture was stirred at ambient temperature overnight. The reaction mixture was filtered and the filtrate was concentrated in vacuo. The residue was washed with cold water to give 2-amino-4-bromo-5-fluorophenol (38.0 g, crude) which was used in the next step directly without further purification. 1H NMR (DMSO-d6, 400 MHz): δ 9.82 (br s, 1H), δ 6.76 (d, J=7.2 Hz, 1H), 6.60 (d, J=10.0 Hz, 1H), 4.65 (br s, 2H).
후처리
- filtrationThe reaction mixture was filtered
- concentrationthe filtrate was concentrated in vacuo
- washThe residue was washed with cold water
출처 및 근거
- ORD 기록
- ord-464d4b35829c4d1c86b0eefba09e1502
- 출처 데이터셋
- uspto-grants-2015_08
- 특허 번호
- US09115151B2
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