반응 #75434
ord-a762b41f09c1473cb4356d6a9dbef19b
반응 방정식
Sodium bicarbonate
dimethylallyl bromide
2-nitroimidazole
→
N-(Dimethylallyl)-2-nitroimidazole
반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1온도under reflux for 16 hours
- 2기타The solvent was removed under reduced pressure
- 3workup.DISSOLUTIONthe residue was dissolved in ethyl acetate
- 4여과The solution was filtered
- 5건조dried with anhydrous sodium sulfate
- 6기타Removal of the solvent
- 7기타gave an oil which
- 8기타was recrystallized from petroleum ether (35-50° C.)
실험 절차
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).