Imidazole → 4-Chloro-6-(1H-imidazol-1-yl)pyrimidine
반응식
Cl[C:2]1[CH:7]=[C:6]([Cl:8])[N:5]=[CH:4][N:3]=1.[NH:9]1[CH:13]=[CH:12][N:11]=[CH:10]1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C.O>[Cl:8][C:6]1[CH:7]=[C:2]([N:9]2[CH:13]=[CH:12][N:11]=[CH:10]2)[N:3]=[CH:4][N:5]=1참가 물질
6
실험 절차
A mixture of 4,6-dichloropyrimidine (5 g, 33.56 mmol), imidazole (2.28 g, 33.56 mmol) and potassium carbonate (4.63 g, 33.56 mmol) in DMF (50 ml) is stirred at room temperature over night. The mixture is diluted with four volumes of water and extracted with dichloromethane. The organic extract is concentrated under reduced pressure and eluted through silica gel with a mixture of ethyl acetate and methanol (9:1). Evaporation of solvent and trituration of the residue with a mixture of diethyl ether and petroleum ether (1:1) leaves 15b (4.07 g, 67%). Mp 198-200° C.
후처리
- extractionextracted with dichloromethane
- extractionThe organic extract
- concentrationis concentrated under reduced pressure
- washeluted through silica gel with a mixture of ethyl acetate and methanol (9:1)
- customEvaporation of solvent and trituration of the residue
- additionwith a mixture of diethyl ether and petroleum ether (1:1)
출처 및 근거
- ORD 기록
- ord-d8e70efc20384575b75fc991697afd85
- 출처 데이터셋
- uspto-grants-1999_07
- 특허 번호
- US05922724
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