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 mixture was refluxed overnight and the solvent was then distilled off under reduced pressure. To the residue was added chloroform and the insoluble matter was filtered off. The solvent was 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 mixture was refluxed overnight
2. distillationthe solvent was then distilled off under reduced pressure
3. additionTo the residue was added chloroform
4. filtrationthe insoluble matter was filtered off
5. distillationThe solvent was distilled off
6. customthe residue was purified by silica gel chromatography (eluent: chloroform:methanol=10:1)