Sodium Dithionite → 2-Amino-4-bromo-5-fluorophenol
반응식
[O-]S(S([O-])=O)=O.[Na+].[Na+].[Br:9][C:10]1[C:15]([F:16])=[CH:14][C:13]([OH:17])=[C:12]([N+:18]([O-])=O)[CH:11]=1>O.C(O)C>[NH2:18][C:12]1[CH:11]=[C:10]([Br:9])[C:15]([F:16])=[CH:14][C:13]=1[OH:17]참가 물질
5
실험 절차
A suspension of Na2S2O4 (51.6 g, 296 mmol) in water (122 mL) was added slowly to a refluxed mixture of 4-bromo-5-fluoro-2-nitrophenol (14 g, 59.3 mmol) in ethanol (1000 mL). The resulting mixture was refluxed for 1 h. After cooling down the salts were filtered off and the filtrate was partially concentrated. Brine was added, extracted with diethyl ether, the extract dried and concentrated to give the crude title compound which was used without further purification (9.2 g, 75%). 1H-NMR (400 MHz, DMSO) 4.65 (br, 2H), 6.60 (d, J=11.3, 1H), 6.76 (d, J=7.8, 1H), 9.80 (br, 1H).
후처리
- temperatureThe resulting mixture was refluxed for 1 h
- temperatureAfter cooling down the salts
- filtrationwere filtered off
- concentrationthe filtrate was partially concentrated
- additionBrine was added
- extractionextracted with diethyl ether
- customthe extract dried
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-bcab26d2617248f698acdfe409a66792
- 출처 데이터셋
- uspto-grants-2011_08
- 특허 번호
- US07989442B2
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