Acetic Acid → 2-Bromo-4-fluoro-(methyloxy)aniline
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CO[C:3]1[CH:8]=[C:7]([N+:9]([O-])=[O:10])[C:6]([Br:12])=[CH:5][C:4]=1[F:13].[C:14](O)(=O)C.C(O)C.C(=O)([O-])[O-].[K+].[K+]>O.[Fe]>[Br:12][C:6]1[CH:5]=[C:4]([F:13])[CH:3]=[CH:8][C:7]=1[NH:9][O:10][CH3:14]참가 물질
7
실험 절차
A mixture of 4-bromo-2-fluoro-5-nitrophenyl methyl ether (25.5 g, 102 mmol), acetic acid (250 mL), ethanol (250 mL) and iron powder (22.7 g, 408 mmol) was heated to 100 C for 4 hours. The reaction mixture was cooled to room temperature, diluted with water, neutralised by addition of potassium carbonate and filtered through Celite. The aqueous layer was extracted thrice with DCM. The combined organic layers were dried over magnesium sulfate and evaporated under vacuum to afford the title compound (15 g, 67%) as a white solid. LC-MS (ES) (M+H)+ m/z=220.
후처리
- temperaturewas heated to 100 C for 4 hours
- filtrationfiltered through Celite
- extractionThe aqueous layer was extracted thrice with DCM
- dry with materialThe combined organic layers were dried over magnesium sulfate
- customevaporated under vacuum
출처 및 근거
- ORD 기록
- ord-4580695b6e6a478b8f5e304c89b48a1d
- 출처 데이터셋
- uspto-grants-2010_04
- 특허 번호
- US07691850B2
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