反应详情

A mixture of 2-chloro-4-nitro-1H-imidazole (8.39 g, 56.88 mmol), tert-butyl 4-(2-methyloxiran-2-ylmethyl)homopiperazine-1-carboxylate (15.38 g, 56.88 mmol) and sodium acetate (5.13 g, 62.57 mmol) in 1-propanol (100 ml) was stirred under reflux for 10 hours. The reaction mixture was allowed to return to room temperature and then concentrated under reduced pressure. The residue was dissolved in methylene chloride. The solution was washed with water, dried over sodium sulfate and then filtered. The filtrate was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (methylene chloride/ethyl acetate=5/1) to afford tert-butyl 4-[3-(2-chloro-4-nitroimidazol-1-yl)-2-hydroxy-2-methylpropyl]homopiperazine-1-carboxylate (6.25 g, yield 27%) as a reddish yellow oil.

1. temperatureunder reflux for 10 hours
2. customto return to room temperature
3. concentrationconcentrated under reduced pressure
4. dissolutionThe residue was dissolved in methylene chloride
5. washThe solution was washed with water
6. dry with materialdried over sodium sulfate
7. filtrationfiltered
8. concentrationThe filtrate was concentrated under reduced pressure
9. customthe residue was purified by silica gel column chromatography (methylene chloride/ethyl acetate=5/1)