反应详情

温度

25 °C

A mixture of 4-[2-(2,2,2-trifluoroethoxy)phenyl]piperazine (2.37 g, 9.1 mmol), 1-bromo-3-chloropropane (14.34 g, 9 mL, 91.1 mmol), potassium carbonate (1.88 g, 13.6 mmol) and acetonitrile (40 mL) was heated 16 hours at reflux under argon. The reaction mixture was allowed to cool to 25° C., then filtered and concentrated in vacuo. The residue was further concentrated at 60° C. in vacuo to remove excess 1-bromo-3-chloropropane. The residue was purified by flash chromatography on silica gel eluting with hexane/ethyl acetate (1:1) to give a mixture of 1-chloro- and 1-bromo-3-{4-[2-(2,2,2-trifluoroethoxy)phenyl]piperazin-1-yl}propane (1.4 g).

1. temperaturewas heated 16 hours
2. temperatureat reflux under argon
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. concentrationThe residue was further concentrated at 60° C. in vacuo
6. customto remove excess 1-bromo-3-chloropropane
7. customThe residue was purified by flash chromatography on silica gel eluting with hexane/ethyl acetate (1:1)
8. customto give