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[CH2:1]([O:3][C:4](=[O:19])/[CH:5]=[C:6](/[O:8][C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([C:15]([F:18])([F:17])[F:16])[CH:10]=1)\[CH3:7])[CH3:2].[Br:20]N1C(=O)CCC1=O.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1>C(Cl)(Cl)(Cl)Cl>[CH2:1]([O:3][C:4](=[O:19])/[CH:5]=[C:6](/[O:8][C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([C:15]([F:16])([F:18])[F:17])[CH:10]=1)\[CH2:7][Br:20])[CH3:2]참가 물질
실험 절차
To a stirred mixture of (E)-3-(3-trifluoromethyl-phenoxy)-but-2-enoic acid ethyl ester (5.33 g, 0.019 mol) in carbon tetrachloride (30 mL) under a nitrogen atmosphere was added N-bromosuccinimide (5.20 g, 0.029 mol) and benzoyl peroxide (470 mg, 0.002 mol). Nitrogen gas was bubbled through the mixture for 5 min, and the resulting mixture was heated to reflux for 4 h. The reaction mixture was then placed in the refrigerator overnight. The solids formed were removed by filtration and the filtrate concentrated in vacuo. The crude product obtained was purified using flash column chromatography (silica gel (100-200 mesh), ethyl acetate/hexanes) to afford (E)-4-bromo-3-(3-trifluoromethyl-phenoxy)-but-2-enoic acid ethyl ester (3.80 g, 55%) as a yellow oil.
후처리
- customNitrogen gas was bubbled through the mixture for 5 min
- temperaturethe resulting mixture was heated
- temperatureto reflux for 4 h
- customwas then placed in the refrigerator overnight
- customThe solids formed
- customwere removed by filtration
- concentrationthe filtrate concentrated in vacuo
- customThe crude product obtained
- customwas purified
출처 및 근거
- ORD 기록
- ord-89b830132c7d4d35857e2545e6a12ca4
- 출처 데이터셋
- uspto-grants-2010_06
- 특허 번호
- US07741327B2
연결된 노트
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