反应详情

2-Chloro-4-nitro-1H-imidazole (3.19 g, 21.6 mmol) and tert-butyl 4-(2-methyloxiran-2-ylmethyl)-piperazine-1-carboxylate (5.53 g, 21.6 mmol) and sodium acetate (1.95 g, 23.8 mmol) were dissolved in 1-propanol (50 ml) followed by stirring under reflux for 48 hours. The reaction mixture was diluted with methylene chloride. The solution was washed with water and a saturated saline solution, dried over sodium sulfate and then filtered. The filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (methylene chloride/methanol=100/1) and treated with methylene chloride-diisopropyl ether to afford 2-(4-tert-butoxycarbonylpiperazin-1-yl)methyl-2-methyl-6-nitro-2,3-dihydroimidazo[2,1-b]oxazole (1.85 g, yield 23%) as a white powder.

1. temperatureunder reflux for 48 hours
2. washThe solution was washed with water
3. dry with materiala saturated saline solution, dried over sodium sulfate
4. filtrationfiltered
5. concentrationThe filtrate was concentrated under reduced pressure
6. customThe residue was purified by silica gel column chromatography (methylene chloride/methanol=100/1)
7. additiontreated with methylene chloride-diisopropyl ether