反应详情

A mixture of 15.6 g (0.35 mole) of 4'-fluoro-5-[4-(α-hydroxy-α-phenylbenzyl)piperidino]valerophenone, the free base of the compound of Example 2, and a small amount of potassium iodide in 100 ml of piperidine is refluxed for about 22 hours. The unreacted piperidine is removed under vacuum, and the remaining residue is triturated with water. The water is decanted and the residue is dissolved in methanol and then added to a large amount of water. The resulting precipitate is dissolved in a large volume of ether, dried over magnesium sulfate, and filtered. The filtrate is concentrated and cooled yielding a product which is recrystallized from ether to give 5-[4-(α-hydroxy-α-phenylbenzyl)piperidino]-4'-piperidinovalerophenone.

1. customThe unreacted piperidine is removed under vacuum
2. customthe remaining residue is triturated with water
3. customThe water is decanted
4. dissolutionthe residue is dissolved in methanol
5. additionadded to a large amount of water
6. dissolutionThe resulting precipitate is dissolved in a large volume of ether
7. dry with materialdried over magnesium sulfate
8. filtrationfiltered
9. concentrationThe filtrate is concentrated
10. temperaturecooled
11. customyielding a product which
12. customis recrystallized from ether