反应详情

温度

120 °C

A sealed tube was charged with 4-nitro-1H-imidazole (500 mg, 4.42 mmol), 3-iodooxetane (920 mg, 5.0 mmol), Cs2CO3 (2.90 g, 8.84 mmol), and dioxane (12 mL). The sealed tube was heated at 120° C. for 16 h. It was then cooled to room temperature and filtered. The filtrate was evaporated under reduced pressure. The residue was purified by silica-gel column chromatography eluting with 30:1 dichloromethane/methanol to afford 285a as a white solid (250 mg, 33%). MS-ESI: [M+H]+ 170.2.

1. temperatureIt was then cooled to room temperature
2. filtrationfiltered
3. customThe filtrate was evaporated under reduced pressure
4. customThe residue was purified by silica-gel column chromatography
5. washeluting with 30:1 dichloromethane/methanol