反应详情

1.2 g (2.49 mMol) of 1-methyl-2-[N-(4-cyanophenyl)-aminomethyl]-benzimidazol-5-yl-carboxylic acid-N-phenyl-N-(2-ethoxycarbonylethyl)-amide were stirred in 100 ml of saturated ethanolic hydrochloric acid for 6 hours at room temperature. Then the mixture was evaporated to dryness in vacuo, the residue was dissolved in 100 ml of ethanol, mixed with 2.5 g (26 mMol) of ammonium carbonate and stirred overnight at room temperature. After distillation of the solvent the crude product thus obtained was purified by column chromatography (100 g silica gel; eluant: dichloromethane/ethanol=4:1). By concentrating the eluates the desired compound was obtained as a white, amorphous solid. Yield: 1.10 g (83% of theory), Rf value: 0.18 (silica gel; dichloromethane/ethanol=4:1) C28H30N6O3 ×HCl (498.6) ##EQU8##

1. customThen the mixture was evaporated to dryness in vacuo
2. dissolutionthe residue was dissolved in 100 ml of ethanol
3. distillationAfter distillation of the solvent the crude product
4. customthus obtained
5. customwas purified by column chromatography (100 g silica gel; eluant: dichloromethane/ethanol=4:1)
6. concentrationBy concentrating the eluates the desired compound
7. customwas obtained as a white, amorphous solid