3-Fluoro-4-nitrophenol → 4-Amino-3-fluorophenol
반응식
[F:1][C:2]1[CH:3]=[C:4]([OH:11])[CH:5]=[CH:6][C:7]=1[N+:8]([O-])=O.C(O[K])=O>C1COCC1.O.[Pd]>[NH2:8][C:7]1[CH:6]=[CH:5][C:4]([OH:11])=[CH:3][C:2]=1[F:1]참가 물질
5
반응 조건
- 온도
- 50 °C
실험 절차
A suspension of 3-fluoro-4-nitrophenol (2.0 g, 12.73 mmol), 10% Pd/C (0.4 g) and HCOOK (8.75 g, 101.85 mmol) in THF/H2O (70 mL/20 mL) was stirred at 50° C. for 5 hours, then cooled to rt, and filtered through CELITE®. The filtrate was diluted with water (30 mL) and extracted with THF (50 mL). The organic layer was dried over Na2SO4 and concentrated in vacuo. The residue was diluted with water (50 mL) and extracted with DCM (50 mL). The organic layer was dried over anhydrous Na2SO4 and concentrated in vacuo to give the title compound as a brown solid (1.17 g, 72.3%).
후처리
- temperaturecooled to rt
- filtrationfiltered through CELITE®
- additionThe filtrate was diluted with water (30 mL)
- extractionextracted with THF (50 mL)
- dry with materialThe organic layer was dried over Na2SO4
- concentrationconcentrated in vacuo
- additionThe residue was diluted with water (50 mL)
- extractionextracted with DCM (50 mL)
- dry with materialThe organic layer was dried over anhydrous Na2SO4
- concentrationconcentrated in vacuo
출처 및 근거
- ORD 기록
- ord-ce6b1edf87cc4a6695d4e06fe3070df3
- 출처 데이터셋
- uspto-grants-2016_05
- 특허 번호
- US09326975B2
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