反应详情

Under an ice-cooling condition, sodium hydride (3.56 g) was added to a N,N-dimethylformamide (100 ml) solution of 2,5-dibromo-4-nitroimidazole (20.08 g). 10 minutes later, being added dropwise chloromethylmethyl ether (6.75 ml) thereto at 10 to 15° C., then the reaction mixture was turned back to a room temperature. After being stirred this reaction mixture for 5 hours, under an ice-cooling condition, sodium hydride (0.30 g) and chloromethylmethyl ether (0.56 ml) were added, further stirred at a room temperature for 1 hour. Then the reaction mixture was ice-cooled, water was added and extracted with ethyl acetate. The organic layer was washed with an aqueous solution being saturated with sodium chloride, dried over anhydrous sodium sulfate, then concentrated under a reduced pressure. Thus obtained crude crystals were washed with diisopropyl ether, and dried at 50° C. for 24 hours, there was obtained 2,5-dibromo-1-methoxymethyl-4-nitroimidazole (19.68 g, yield: 84.3%) as yellow powder product.

1. customat 10 to 15° C.
2. customwas turned back to a room temperature
3. additionwere added
4. stirringfurther stirred at a room temperature for 1 hour
5. temperaturecooled
6. extractionextracted with ethyl acetate
7. washThe organic layer was washed with an aqueous solution
8. dry with materialdried over anhydrous sodium sulfate
9. concentrationconcentrated under a reduced pressure
10. customThus obtained crude crystals
11. washwere washed with diisopropyl ether
12. customdried at 50° C. for 24 hours