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
In THF (15ml) was dissolved N-[4-(chloromethyl)-phenyl]-7-(4-methylphenyl)-3,4-dihydronaphthalene-2-carboxamide (300mg), and to the mixture was added 4-benzylpiperidine (408 μl). The mixture was refluxed for 19 hours. The reaction mixture was cooled to room temperature, and to the mixture was added water (100ml). The mixture was extracted with ethyl acetate. The organic layer was washed with saturated sodium chloride solution, dried with anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was separated and purified with column chromatography (ethyl acetate) and recrystallized from ethyl acetate-hexane to give N-[4-(4-benzyl-piperidinomethyl)-phenyl]-7-(4-methylphenyl)-3,4-dihydronaphthalene-2-carboxamide (Compound 35) (259mg) as colorless crystals.
WORKUP
后处理
- temperatureThe mixture was refluxed for 19 hours
- extractionThe mixture was extracted with ethyl acetate
- washThe organic layer was washed with saturated sodium chloride solution
- dry with materialdried with anhydrous sodium sulfate
- concentrationconcentrated under reduced pressure
- customThe residue was separated
- custompurified with column chromatography (ethyl acetate)
- customrecrystallized from ethyl acetate-hexane