191602-52-5 → HCID 18787114、化合物
反応式
[Br:1][C:2]1[C:10]2[O:9][CH2:8][CH2:7][C:6]=2[CH:5]=[C:4]([N+:11]([O-])=O)[CH:3]=1>C(O)(=O)C.O.[Fe]>[NH2:11][C:4]1[CH:3]=[C:2]([Br:1])[C:10]2[O:9][CH2:8][CH2:7][C:6]=2[CH:5]=1参加物
5
実験手順
7-Bromo-5-nitro-2,3-dihydrobenzofuran (2 g) was suspended in acetic acid (5 ml) and water (12 ml). Iron powder (3.5 g) was added and the mixture was heated at reflux for 3hr. The cooled mixture was cooled and filtered through celite. The filtrate was concentrated and azeotroped with toluene. The residue was purified by chromatography on silica using 10% ethyl acetate in hexane as eluent to afford the title compound (1.3 g) as an oil. 1H NMR (250 MHz, CDCl3) δ 3.22 (2H, t, J=7.5 Hz), 3.38 (2H, br s), 4.58 (2H, t, J=8 Hz), 6.51-6.53 (1H, m), 6.63-6.64 (1H, m).
後処理
- temperaturethe mixture was heated
- temperatureat reflux for 3hr
- temperatureThe cooled mixture was cooled
- filtrationfiltered through celite
- concentrationThe filtrate was concentrated
- customazeotroped with toluene
- customThe residue was purified by chromatography on silica using 10% ethyl acetate in hexane as eluent
出典と根拠
- ORDレコード
- ord-1e4f8a0da8514f27a0ef2c8064418f22
- 出典データセット
- uspto-grants-2000_05
- 特許番号
- US06060469
反応ノート
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