反应详情

To a solution of 2-[2-(dimethylamino)ethylamino]-4-nitro-1H-benzimidazole (105 mg) in ethanol (4 ml) were added iron (reduced, 118 mg) and acetic acid (0.24 ml) at room temperature and the mixture was refluxed for 6 hours. The precipitate was filtered off and the filtrate was evaporated in vacuo. The residue was dissolved in a mixture of chloroform and methanol (5-1) and the organic layer was washed with saturated aqueous sodium hydrogencarbonate solution, and dried over magnesium sulfate. The solvent was evaporated in vacuo. The residue was purified by preparative thin-layer chromatography (chloroform-methanol-ammonia solution (28%)=160-32-1) to give 4-amino-2-[2-(dimethylamino)-ethylamino]-1H-benzimidazole (80 mg).

1. temperaturethe mixture was refluxed for 6 hours
2. filtrationThe precipitate was filtered off
3. customthe filtrate was evaporated in vacuo
4. dissolutionThe residue was dissolved in a mixture of chloroform and methanol (5-1)
5. washthe organic layer was washed with saturated aqueous sodium hydrogencarbonate solution
6. dry with materialdried over magnesium sulfate
7. customThe solvent was evaporated in vacuo
8. customThe residue was purified by preparative thin-layer chromatography (chloroform-methanol-ammonia solution (28%)=160-32-1)