HRID1079395
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of N-(4-aminophenyl)piperidine dihydrochloride obtained in Example 17 and 1-acetyl-4-piperidone (0.70 g) in methanol (10 ml) was added sodium cyano borohydride (0.63 g), followed by stirring at room temperature for 5 hours. To the mixture was added ethyl acetate ester (20 ml) and water (30 ml). After the organic layer was dried over anhydrous sodium sulfate, to the solution was added 6N solution of hydrogen chloride in dioxane (2 ml) and the solvent was distilled off. The residue was recrystallized from ethanol to obtain colorless crystals, m.p. 187°-193° C.
WORKUP
后处理
- dry with materialAfter the organic layer was dried over anhydrous sodium sulfate, to the solution
- additionwas added 6N solution of hydrogen chloride in dioxane (2 ml)
- distillationthe solvent was distilled off
- customThe residue was recrystallized from ethanol
- customto obtain colorless crystals, m.p. 187°-193° C.