反应详情

A mixture of 1-[1-{4-[3-(N-benzyl-N-methylamino)-propoxy] benzoyl}-4-piperidinyl]-3,4-dihydrocarbostyril (5.3 g), 5% palladium-carbon (0.8 g), ammonium formate (2.6 g) and ethanol (300 ml) is refluxed with heating for 2 hours. The catalyst is filtered off and ethanol is distilled off under reduced pressure. To the residue is added chloroform and the mixture is washed successively with saturated sodium hydrogen carbonate, water and saline solution. Further the mixture is dried with sodium sulfate and the solvent is distilled off. The resulting residue is purified by silica gel column chromatography (solvent: dichloromethane:methanol=20:1→5:1) to give 1-[1-{4-[3-(N-methylamino)propoxy]benzoyl}-4-piperidinyl]-3,4-dihydrocarbostyril (4.37 g).

1. temperatureis refluxed
2. temperaturewith heating for 2 hours
3. filtrationThe catalyst is filtered off
4. distillationethanol is distilled off under reduced pressure
5. additionTo the residue is added chloroform
6. washthe mixture is washed successively with saturated sodium hydrogen carbonate, water and saline solution
7. dry with materialFurther the mixture is dried with sodium sulfate
8. distillationthe solvent is distilled off
9. customThe resulting residue is purified by silica gel column chromatography (solvent: dichloromethane:methanol=20:1→5:1)