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, 3.6 g (0.018 mol) of (3-bromopropyl) benzene (G.O. Aspinall et al., J.Chem.Soc.1950, 743) was added dropwise at room temperature. The mixture was then slowly heated and refluxed for 3 hours. The reaction mixture was filtered and the filtrate was concentrated. The residue was taken up in diethyl ether, undissolved matter was filtered off and ethereal maleic acid was added until the liquid reacted acidic. The precipitate was filtered off and crystallized from a mixture of methanol and dimethylformamide. 1-[2-[Bis(4-fluorophenyl)methoxy]ethyl]-4-(3-phenylpropyl)piperazine maleate (1:2) was obtained. Melting point 185.0°-185.5° C.

1. additionwas added dropwise at room temperature
2. temperatureThe mixture was then slowly heated
3. temperaturerefluxed for 3 hours
4. filtrationThe reaction mixture was filtered
5. concentrationthe filtrate was concentrated
6. filtrationundissolved matter was filtered off
7. additionethereal maleic acid was added until the liquid
8. customreacted acidic
9. filtrationThe precipitate was filtered off
10. customcrystallized from a mixture of methanol and dimethylformamide