反应详情

To a solution of N-(3-aminophenyl)piperidine dihydrochloride (3.73 g) and 1-acetyl-4-piperidone (2.1 g) in methanol (30 ml) was added sodium cyano borohydride (1.9 g), followed by stirring at room temperature for 5 hours. To the mixture were added ethyl acetate ester (20 ml) and water (30 ml), the organic layer was dried over anhydrous sodium sulfate and then the solvent was distilled off. The residual oily compound was separated and purified by silica gel column chromatography (developing solvent: ethyl acetate ester). The oily compound was dissolved in dioxane (10 ml) and to the mixture was added 6N solution of hydrogen chloride in dioxane (2 ml). Then, the solvent was removed to obtain a colorless amorphous solid (3.7 g).

1. dry with materialthe organic layer was dried over anhydrous sodium sulfate
2. distillationthe solvent was distilled off
3. customThe residual oily compound was separated
4. custompurified by silica gel column chromatography (developing solvent: ethyl acetate ester)
5. dissolutionThe oily compound was dissolved in dioxane (10 ml) and to the mixture
6. additionwas added 6N solution of hydrogen chloride in dioxane (2 ml)
7. customThen, the solvent was removed