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To 14.32 g (60 mmol) of said 4,4'-difluorobenzhydryl chloride were added 10.46 g (90 mmol) of anhydrous sodium carbonate, 25.84 g (300 mmol) of piperazine and 52 ml of dry chloroform, and the mixture was heated under reflux. To the reaction mixture was added dropwise over 45 minutes 14.32 g (60 mmol) of 4,4'-difluorobenzhydryl chloride in 13 ml of dry chloroform. The mixture was heated under reflux for 18 hours and filtered. The filtrate was washed successively with water and a saturated aqueous sodium chloride solution, and the organic layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure. There was obtained a residue, which was subjected to column chromatography on silica gel to give 13.49 g (47 mmol) of 4,4'-difluorobenzhydryl piperazine from eluates of dichloromethane-methanol (10:1).

1. temperaturethe mixture was heated
2. temperatureunder reflux
3. temperatureThe mixture was heated
4. temperatureunder reflux for 18 hours
5. filtrationfiltered
6. washThe filtrate was washed successively with water
7. dry with materiala saturated aqueous sodium chloride solution, and the organic layer was dried over anhydrous sodium sulfate
8. concentrationconcentrated under reduced pressure
9. customThere was obtained a residue, which