反应详情

A mixture of 4-nitro-imidazole (2.75 g, 24.3 mmol), benzyl chloride (4.3 g, 26.8 mmol), potassium carbonate (4 g, 29.2 mmol), and acetonitrile (50 mL) was stirred for 2 h at rt, warmed to 55° C., stirred for 16 h, allowed to cool to rt, concentrated, diluted with water, and extracted with EtOAc. The organic extracts were washed with brine, dried (Na2SO4), filtered, and concentrated. The residue was purified by silica gel column chromatography (hexane/EtOAc, 4:1) to afford 5.6 g of the title compound. tR: 0.93 min (LC-MS 4); ESI-MS: 234.3 [M+H]+ (LC-MS 4); Rf=0.25 (hexane/EtOAc, 4:1).

1. temperaturewarmed to 55° C.
2. stirringstirred for 16 h
3. temperatureto cool to rt
4. concentrationconcentrated
5. additiondiluted with water
6. extractionextracted with EtOAc
7. washThe organic extracts were washed with brine
8. dry with materialdried (Na2SO4)
9. filtrationfiltered
10. concentrationconcentrated
11. customThe residue was purified by silica gel column chromatography (hexane/EtOAc, 4:1)