反应详情

A mixture of 25 g of 2-bromo-2'-methylpropiophenone, 70 ml of dry acetonitrile, 30 g of potassium carbonate and 19 g of 4-benzylpiperidine is stirred for 4 hours at ambient temperature. It is filtered in order to separate off the inorganic residue, and the filtrate is diluted with 200 ml of diethyl ether, which causes precipitation of 4-benzylpiperidine hydrobromide. This is filtered off; the filtrate deposits a second crop of hydrobromide, which is also separated off. The filtrate is then acidified with 300 ml of 3N hydrochloric acid. The intermediate propiophenone hydrochloride is an oil which is insoluble in both phases. The acid aqueous phase is extracted twice with methylene chloride, the extract is washed with water, and aqueous ammonia solution is added. The mixture is stirred and left to separate, the organic phase is dried, filtered and treated with about 100 g of silica in order to retain the traces of 4-benzylpiperidine, the mixture is filtered and the filtrate is evaporated. 10.9 g of an oil are collected.

1. filtrationIt is filtered in order
2. customto separate off the inorganic residue
3. additionthe filtrate is diluted with 200 ml of diethyl ether, which
4. customprecipitation of 4-benzylpiperidine hydrobromide
5. filtrationThis is filtered off
6. customthe filtrate deposits a second crop of hydrobromide, which is also separated off
7. extractionThe acid aqueous phase is extracted twice with methylene chloride
8. washthe extract is washed with water, and aqueous ammonia solution
9. additionis added
10. stirringThe mixture is stirred
11. waitleft
12. customto separate
13. customthe organic phase is dried
14. filtrationfiltered
15. additiontreated with about 100 g of silica in order
16. filtrationthe mixture is filtered
17. customthe filtrate is evaporated
18. custom10.9 g of an oil are collected