反应 #75434
ord-a762b41f09c1473cb4356d6a9dbef19b
反应方程式
Sodium bicarbonate
dimethylallyl bromide
2-nitroimidazole
→
N-(Dimethylallyl)-2-nitroimidazole
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1温度under reflux for 16 hours
- 2其他The solvent was removed under reduced pressure
- 3workup.DISSOLUTIONthe residue was dissolved in ethyl acetate
- 4过滤The solution was filtered
- 5干燥dried with anhydrous sodium sulfate
- 6其他Removal of the solvent
- 7其他gave an oil which
- 8其他was recrystallized from petroleum ether (35-50° C.)
实验过程
Sodium bicarbonate (0.42 g, 50 mmol) and dimethylallyl bromide (3.28 g, 22 mmol) were added to a suspension of 2-nitroimidazole (2.26 g, 20 mmol) in dry acetonitrile (10 mL). The mixture was stirred under reflux for 16 hours. The solvent was removed under reduced pressure, and the residue was dissolved in ethyl acetate. The solution was filtered, and dried with anhydrous sodium sulfate. Removal of the solvent gave an oil which was recrystallized from petroleum ether (35-50° C.). Yield 1.83 g, m.p. 48-49° C. 1H NMR (CDCl3) δ7.24 (s, 1H), 7.22 (s, 1H), 5.46 (m, 1H), 5.1 (d, 2H), 1.91 (s, 3H) and 1.90 (s, 3H).