反应详情

In ethanol (100 ml) was dissolved sodium metal (0.70 g) followed by addition of a solution of N-(2-ethoxycarbonylaminophenyl)-N-ethoxycarbonyl-N',N'-dimethylethylenediamine (4.88 g) in ethanol (20 ml). The reaction mixture was refluxed for 16 hours and was concentrated under reduced pressure. The residue was diluted with chloroform and the insoluble matter was filtered off. The solvent was then distilled off and the residue was purified by silica gel chromatography (eluent:chloroform:methanol=10:1) to give 2.69 g of 1,3-dihydro-1-(2-dimethylaminoethyl)-2H-benzimidazol-2-one.

1. temperatureThe reaction mixture was refluxed for 16 hours
2. concentrationwas concentrated under reduced pressure
3. additionThe residue was diluted with chloroform
4. filtrationthe insoluble matter was filtered off
5. distillationThe solvent was then distilled off
6. customthe residue was purified by silica gel chromatography (eluent:chloroform:methanol=10:1)