反应详情

温度

175 °C

A mixture of 2,3-diaminotoluene (2.0 g) and ethyl N-methyloxamate (2.36 g) in N,N-dimethylformamide (10 ml) was stirred at 175° C. for 8 hours. After being cooled to ambient temperature, the mixture as poured into a mixture of saturated aqueous sodium bicarbonate solution and ethyl acetate and the organic layer was separated. The organic layer was washed with brine and the solution was dried over magnesium sulfate. The solvent was evaporated in vacuo and the residue was chromatographed on silica gel eluting with a mixtue of chloroform and methanol (50:1) to give 4-methyl-2-(N-methylcarbamoyl)-1H-benzimidazole (1.17 g) as a powder.

1. temperatureAfter being cooled to ambient temperature
2. customthe organic layer was separated
3. washThe organic layer was washed with brine
4. dry with materialthe solution was dried over magnesium sulfate
5. customThe solvent was evaporated in vacuo
6. customthe residue was chromatographed on silica gel eluting with a mixtue of chloroform and methanol (50:1)