反应详情

Sodium bicarbonate (2.9 g) was added to a solution of 1-(2-chloroethyl)imidazole (4.0 g) and 4-(3-phenylpropyl)piperidine (6.2 g) in industrial methylated spirits (100 ml) and the reaction mixture heated under reflux for 96 hours. The reaction mixture was then filtered and the filtrate concentrated to give an oil, which was purified by flash chromatography eluting with ethylacetate/methanol/triethylamine (88:10:2). The solid obtained was dissolved in ether, ethereal hydrogen chloride acid was added and the solid precipitated was collected and recrystallised from ethanol/ether to give 1-[2-(imidazol-1-yl)ethyl]-4-(3-phenylpropyl)piperidine, dihydrochloride monohydrate, m.p. 178°-179° C.

1. temperaturethe reaction mixture heated
2. temperatureunder reflux for 96 hours
3. filtrationThe reaction mixture was then filtered
4. concentrationthe filtrate concentrated
5. customto give an oil, which
6. customwas purified by flash chromatography
7. washeluting with ethylacetate/methanol/triethylamine (88:10:2)
8. customThe solid obtained
9. customthe solid precipitated
10. customwas collected
11. customrecrystallised from ethanol/ether