反应详情

A mixture of 1.9 g (0.01 mole) of 3-(3-methoxyphenyl)piperidine, 4.0 g (3.3 ml, 0.02 mole) of 4-oxo-4-(4-fluorophenyl)butyl chloride, 27.6 g (0.20 mole) of potassium carbonate and 75 ml of methyl isobutyl ketone was heated under reflux for ca. 40 hours. The reaction mixture was then poured onto ice-water and the resulting mixture was extracted with ethyl acetate. The combined extracts were washed with water, followed by saturated sodium chloride solution, and then they were dried and evaporated in vacuo. The residue was chromatographed on 250 ml of silica gel, eluting with chloroform/metanol (95:5). The appropriate fractions were combined and evaporated in vacuo to give 1.4 g of the title compound as an amber oil (39% yield).

1. temperaturewas heated
2. temperatureunder reflux for ca. 40 hours
3. additionThe reaction mixture was then poured onto ice-water
4. extractionthe resulting mixture was extracted with ethyl acetate
5. washThe combined extracts were washed with water
6. customthey were dried
7. customevaporated in vacuo
8. customThe residue was chromatographed on 250 ml of silica gel
9. washeluting with chloroform/metanol (95:5)
10. customevaporated in vacuo