反应详情

A mixture of 40 parts of α,α-bis(4-fluorophenyl)-1-(phenylmethyl)-4-piperidinemethanol, 120 parts of a hydrochloric acid solution and 50 parts of acetic acid was stirred and refluxed for 2 hours. The reaction mixture was cooled and water and methylbenzene were added: three layers were obtained. The two supernatant phases were separated and treated with ammonium hydroxide. The organic phase was separated, dried, filtered and evaporated. The residue was crystallized from 2,2'-oxybispropane, yielding 26 parts of 4-[bis(4-fluorophenyl)methylene]-1-(phenylmethyl)piperidine (intermediate 13).

1. temperaturerefluxed for 2 hours
2. temperatureThe reaction mixture was cooled
3. customthree layers were obtained
4. customThe two supernatant phases were separated
5. additiontreated with ammonium hydroxide
6. customThe organic phase was separated
7. customdried
8. filtrationfiltered
9. customevaporated
10. customThe residue was crystallized from 2,2'-oxybispropane