Imidazole → 4-Chloro-6-(1H-imidazol-1-yl)pyrimidine
反応式
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]=1参加物
6
実験手順
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.
後処理
- 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)
出典と根拠
- ORDレコード
- ord-d8e70efc20384575b75fc991697afd85
- 出典データセット
- uspto-grants-1999_07
- 特許番号
- US05922724
反応ノート
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