反应详情

温度

120 °C

In 30 ml of dimethylformamide were dissolved 1.5 g of the above 1:1 (approx.) mixture of Compound h and Compound h', 1.5 g (9.9 mmol) of sodium iodide and 5.0 g (76.3 mmol) of sodium azide and the solution was heated at 120° C. for 48 hours. After cooling, the solvent was distilled off and 50 ml of ethyl acetate was added to the residue. The insolubles were filtered off and the filtrate was washed twice with 5% aqueous sodium thiosulfate solution and, then, three times with saturated aqueous sodium chloride solution. The organic layer was dried over anhydrous magnesium sulfate and the solvent was distilled off under reduced pressure to give 1.38 g (98.9%) of 1-(2-azidoethyl)-2,3-dihydro-2-oxo-1H-benzimidazole (Compound i) as light yellow crystals.

1. temperatureAfter cooling
2. distillationthe solvent was distilled off
3. addition50 ml of ethyl acetate was added to the residue
4. filtrationThe insolubles were filtered off
5. washthe filtrate was washed twice with 5% aqueous sodium thiosulfate solution
6. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
7. distillationthe solvent was distilled off under reduced pressure