Imidazole → 1-(4-Bromo-phenyl)-3-imidazol-1-yl-propan-1-ol
반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([OH:12])[CH2:9][CH2:10]Cl)=[CH:4][CH:3]=1.[NH:13]1[CH:17]=[CH:16][N:15]=[CH:14]1>CN(C)C=O>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([OH:12])[CH2:9][CH2:10][N:13]2[CH:17]=[CH:16][N:15]=[CH:14]2)=[CH:4][CH:3]=1참가 물질
4
실험 절차
A solution of 1-(4-Bromo-phenyl)-3-chloro-propan-1-ol* (1.5 g, 6.01 mmol) and imidazole (1.23 g, 18.03 mmol) in dimethylformamide (18 ml) was heated at 100° C. for 18 hrs then partitioned between water and ethyl acetate. The organic extracts were combined, dried (MgSO4), filtered, concentrated and purified by column chromatography (SiO2), eluting with methanol:dichloromethane (2:98) to methanol:dichloromethane (6:94) to afford the title compound (0.75 g, 44% yield). LC/MS: (PS-B3)Rt 2.48 [M+H]+ 281.14, 283.11.
후처리
- customthen partitioned between water and ethyl acetate
- dry with materialdried (MgSO4)
- filtrationfiltered
- concentrationconcentrated
- custompurified by column chromatography (SiO2)
- washeluting with methanol:dichloromethane (2:98) to methanol:dichloromethane (6:94)
출처 및 근거
- ORD 기록
- ord-3bc4ea4e1c054485bede85cdf5caa2d3
- 출처 데이터셋
- uspto-grants-2012_08
- 특허 번호
- US08247576B2
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