Sodium Dithionite → 2-Amino-4-bromo-5-fluorophenol
反応式
[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]参加物
5
実験手順
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).
後処理
- 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
出典と根拠
- ORDレコード
- ord-bcab26d2617248f698acdfe409a66792
- 出典データセット
- uspto-grants-2011_08
- 特許番号
- US07989442B2
反応ノート
読み込み中…