反应详情

To a mixture of 6 g (0.018 mol) of 1-[2-[bis(4-fluorophenyl)methoxy]ethyl]piperazine (prepared as described in Example 3) and 3 g of potassium carbonate powder in 50 ml of ethanol, 3.1 g (0.018) of benzylbromide were added dropwise at room temperature. The reaction mixture was then slowly heated and refluxed for 3 hours. Subsequently another 3.1 g (0.018 mol) of benzylbromide were added dropwise at room temperature. The mixture was refluxed for 1.5 hours, cooled and filtered. The solvent was distilled off and the residue was purified by column chromatography (silicagel) with a mixture of chloroform and ethyl acetate (1:1) as the eluent. A solution of maleic acid in diethyl ether was added to the desired eluate fraction, the precipitate was filtered off and crystallized from a mixture of methanol and dimethylformamide. 1-[2-[Bis(4-fluorophenyl)methoxy]ethyl]-4-(phenylmethyl)piperazine maleate (1:2) was obtained. Melting point 201.5°-202.5° C.

1. additionwere added dropwise at room temperature
2. temperatureThe reaction mixture was then slowly heated
3. temperaturerefluxed for 3 hours
4. temperatureThe mixture was refluxed for 1.5 hours
5. temperaturecooled
6. filtrationfiltered
7. distillationThe solvent was distilled off
8. customthe residue was purified by column chromatography (silicagel) with a mixture of chloroform and ethyl acetate (1:1) as the eluent
9. additionA solution of maleic acid in diethyl ether was added to the desired eluate fraction
10. filtrationthe precipitate was filtered off
11. customcrystallized from a mixture of methanol and dimethylformamide