HRID1579331
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
A solution of 14.5 g (0.035 mole) of 4-[4-[α-(p-ethylphenyl)benzyl]piperidino]-4'-fluorobutyrophenone in 100 ml of piperidine is refluxed for 22 hours. The unreacted piperidine is removed under vacuum, and the remaining residue is triturated with water. The water is decanted, the residue is dissolved in methanol and added to a large amount of water. The resulting precipitate is dissolved in ether, dried over magnesium sulfate, treated with charcoal and filtered. The filtrate is concentrated to a solid residue and is recrystallized from ethanol-water to give the title compound.
WORKUP
后处理
- customThe unreacted piperidine is removed under vacuum
- customthe remaining residue is triturated with water
- customThe water is decanted
- dissolutionthe residue is dissolved in methanol
- additionadded to a large amount of water
- dissolutionThe resulting precipitate is dissolved in ether
- dry with materialdried over magnesium sulfate
- additiontreated with charcoal
- filtrationfiltered
- concentrationThe filtrate is concentrated to a solid residue
- customis recrystallized from ethanol-water