反应 #2200615

反应方程式

Water

5-bromo-2-fluoro-benzonitrile

4-methylimidazole

potassium carbonate

→

title compound

收率 59.1%

5-Bromo-2-(4-methyl-imidazol-1-yl)-benzonitrile

收率 59.1%

溶剂

DMSO

反应条件

后处理

1. 1
   workup.STIRRINGthe resulting suspension was stirred with ice-bath
2. 2
   温度cooling for 1 h
3. 3
   过滤The precipitate was filtered
4. 4
   洗涤washed with water (0.5 L)
5. 5
   干燥dried at 50° C. over KOH
6. 6
   workup.DISSOLUTIONThe resulting raw material (25.6 g) was dissolved
7. 7
   workup.ADDITIONAfter addition of diisopropylether (300 ml) the solution
8. 8
   温度to cool to room temperature
9. 9
   过滤Filtration
10. 10
    其他drying

实验过程

A mixture of 5-bromo-2-fluoro-benzonitrile (25.0 g, 125 mmol), 4-methylimidazole (12.5 g, 152 mmol), potassium carbonate (34.55 g, 250 mmol) in DMSO (500 mL) was stirred at 90° C. for 16 h. Water (1.5 L) was added and the resulting suspension was stirred with ice-bath cooling for 1 h. The precipitate was filtered, washed with water (0.5 L) and dried at 50° C. over KOH. The resulting raw material (25.6 g) was dissolved in boiling Ethyl acetate (300 ml). After addition of diisopropylether (300 ml) the solution was allowed to cool to room temperature. Filtration and drying afforded the title compound (19.35 g, 59%) as a white solid. Mp 166° C.

来源