反应详情

2-Bromo-5-iodo-4-nitroimidazole (1.00 g, 3.15 mmol) was dissolved in dimethylformamide (8 ml) and water (3 ml). The obtained solution was stirred under cooling on ice, and then, a 50% to 55% ammonium bisulfite aqueous solution (3.6 ml, 23.5 mmol with a content of 52.5%) was added thereto. The obtained mixture was stirred at room temperature for 3 days. Thereafter, cold water (30 ml) was added to the reaction product, followed by extraction with ethyl acetate 3 times (167 ml in total). The organic layer was washed with 5% saline twice and then dried (MgSO4), followed by vacuum concentration and exsiccation.

1. temperatureunder cooling on ice
2. stirringThe obtained mixture was stirred at room temperature for 3 days
3. extractionfollowed by extraction with ethyl acetate 3 times (167 ml in total)
4. washThe organic layer was washed with 5% saline twice
5. dry with materialdried (MgSO4)
6. concentrationfollowed by vacuum concentration and exsiccation