1,4-Dibromobutane → 1-(3-methoxyphenyl)pyrrolidine
반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([NH2:9])[CH:6]=[CH:7][CH:8]=1.Br[CH2:11][CH2:12][CH2:13][CH2:14]Br.C(N(C(C)C)CC)(C)C>C1(C)C=CC=CC=1>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([N:9]2[CH2:14][CH2:13][CH2:12][CH2:11]2)[CH:6]=[CH:7][CH:8]=1참가 물질
5
실험 절차
To a stirring solution of 3-methoxy-phenylamine (571 mg, 4.6 mmol) in anhydrous toluene (40 ml) was added 1,4-dibromo-butane (1.0 g, 4.6 mmol) and diisopropylethylamine (0.59 g, 4.6 mmol). The resulting solution was heated to reflux for 24 hours and then concentrated in vacuo. The crude material was purified by column chromatography over silica gel (silica gel 60, EM science, 5% EtOAc:hexanes) and the title compound was obtained as an oil (754 mg, 92%). MS(ES) m/e 178.4 ([M+H]+).
후처리
- temperatureThe resulting solution was heated
- temperatureto reflux for 24 hours
- concentrationconcentrated in vacuo
- customThe crude material was purified by column chromatography over silica gel (silica gel 60, EM science, 5% EtOAc:hexanes)
출처 및 근거
- ORD 기록
- ord-20689b8aeeea45e7a08ff27b93a3093a
- 출처 데이터셋
- uspto-grants-2008_04
- 특허 번호
- US07365085B2
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