反应详情

1 g of (-)-trans-4-(4-fluorophenyl)-3-(3,4-methylene dioxyphenoxymethyl)-piperidine hydrochloride in 50 ml 99.9% ethanol was mixed with 3-bromopropionitrile (7 ml) and 2 g potassium carbonate. The mixture was refluxed for 70 h. After cooling 25 ml acetone and 25 ml diethylether were added, the precipitate filtered off, and the filtrate evaporated in vacuo. The residue was extracted with 1 N NaOH/ether, the ether layer dried (MgSO4) and evaporated to dryness. The residue was dissolved in acetone and excess conc. HCl was added. Subsequent evaporation gave a hard glass, which was purified on a silica gel column using 99.5% ethanol as eluent. The title compound was isolated, and its structure confirmed by the IR and NMR data. M.p. 156° C.

1. temperatureThe mixture was refluxed for 70 h
2. additionwere added
3. filtrationthe precipitate filtered off
4. customthe filtrate evaporated in vacuo
5. extractionThe residue was extracted with 1 N NaOH/ether
6. dry with materialthe ether layer dried (MgSO4)
7. customevaporated to dryness
8. dissolutionThe residue was dissolved in acetone
9. additionexcess conc. HCl was added
10. customSubsequent evaporation
11. customgave a hard glass, which
12. customwas purified on a silica gel column