反应详情

温度

80 °C

A mixture of alpha-phenyl-4-piperidinemethanol (1.5 g, 7.8 mmol), 2-bromoethyl benzene (1.1 ml, 8.0 mmol) and potassium carbonate (1.1 g, 8.0 mmol) in dry DMF (20 ml) was heated at 80° C. over the weekend (60 h). The excess DMF was distilled off at reduced pressure and the residue was dissolved in ethyl acetate. The organic phase was washed with H2O (3×100 ml), saturated aqueous NaCl (1×100 ml), dried (MgSO4), filtered and evaporated to give a pale yellow oil which eventually crystallized. After recrystallization from ethyl acetate-hexane, a white crystalline solid was obtained, mp 125°-128° C.

1. distillationThe excess DMF was distilled off at reduced pressure
2. dissolutionthe residue was dissolved in ethyl acetate
3. washThe organic phase was washed with H2O (3×100 ml), saturated aqueous NaCl (1×100 ml)
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. customevaporated
7. customto give a pale yellow oil which
8. customeventually crystallized
9. customAfter recrystallization from ethyl acetate-hexane
10. customa white crystalline solid was obtained