反応 #75434

反応方程式

Sodium bicarbonate

dimethylallyl bromide

2-nitroimidazole

→

N-(Dimethylallyl)-2-nitroimidazole

溶媒

acetonitrile

反応条件

後処理

1. 1
   温度under reflux for 16 hours
2. 2
   その他The solvent was removed under reduced pressure
3. 3
   workup.DISSOLUTIONthe residue was dissolved in ethyl acetate
4. 4
   ろ過The solution was filtered
5. 5
   乾燥dried with anhydrous sodium sulfate
6. 6
   その他Removal of the solvent
7. 7
   その他gave an oil which
8. 8
   その他was recrystallized from petroleum ether (35-50° C.)

実験手順

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).

出典