191602-52-5 → HCID 18787114, 화합물
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[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]=1참가 물질
5
실험 절차
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).
후처리
- 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
출처 및 근거
- ORD 기록
- ord-1e4f8a0da8514f27a0ef2c8064418f22
- 출처 데이터셋
- uspto-grants-2000_05
- 특허 번호
- US06060469
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