تفاعل #2200615

معادلة التفاعل

Water

5-bromo-2-fluoro-benzonitrile

4-methylimidazole

potassium carbonate

→

title compound

المردود 59.1%

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

المردود 59.1%

المذيبات

DMSO

ظروف التفاعل

المعالجة

1. 1
   workup.STIRRINGthe resulting suspension was stirred with ice-bath
2. 2
   درجة الحرارةcooling for 1 h
3. 3
   ترشيحThe precipitate was filtered
4. 4
   غسيلwashed with water (0.5 L)
5. 5
   تجفيفdried 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
   درجة الحرارةto cool to room temperature
9. 9
   ترشيحFiltration
10. 10
    أخرىdrying

الإجراء التجريبي

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.

المصدر