反应详情

A mixture of 7.41 g (0.025 mole) of [4-[bis(4-fluorophenyl)methyl]piperidine, 4.90 g (0.025 mole) of 2-(3-chloropropoxy)benzonitrile, and potassium carbonate, 5.54 g (0.04 mole) was heated overnight at reflux in 350 ml of 1-butanol containing potassium iodide (0.2 g). The mixture was concentrated to dryness and the resulting residue was partitioned several times between water and chloroform. The chloroform layer was dried (anhydrous sodium sulfate), filtered, and solvent removed to give a brown oil. The oil was triturated with ethyl ether and placed in a freezer overnight. White crystals were obtained and dried in vacuo overnight at room temperature. A yield of 5.15 g (46.1%) of analytically pure material, m.p. 88.5°-90° C., was obtained.

1. temperaturewas heated overnight
2. concentrationThe mixture was concentrated to dryness
3. customthe resulting residue was partitioned several times between water and chloroform
4. dry with materialThe chloroform layer was dried (anhydrous sodium sulfate)
5. filtrationfiltered
6. customsolvent removed
7. customto give a brown oil
8. customThe oil was triturated with ethyl ether
9. customWhite crystals were obtained
10. customdried in vacuo overnight at room temperature
11. customA yield of 5.15 g (46.1%) of analytically pure material, m.p. 88.5°-90° C., was obtained