反应详情

77 g (0.2685 mole) of levorotatory (-)-1-[(4-chlorophenyl)phenylmethyl]piperazine (prepared in Example 4.1), 40.5 g (0.2932 mole) of 2-(2-chloroethoxy)acetamide, 62.8 g (0.591 mole) of sodium carbonate and 2 g (0.0120 mole) of potassium iodide are added to 700 ml of toluene. The mixture is heated at reflux temperature for 24 hours. 10 g of Norit are then added and the mixture is filtered while hot through Dicalite. The filtrate is washed with 500 ml of water and then with 500 ml of a saturated aqueous solution of sodium chloride. The organic phase is separated and dried over 250 g of sodium sulfate. It is then filtered and 10 the solvent is evaporated. The residual oil is taken up in 1500 ml of hot diisopropyl oxide. The solution is heated under reflux and allowed to crystallize by cooling in an ice bath. The crystals are filtered, washed with a small amount of diisopropyl oxide and dried under vacuum at 40° C. 82.91 g of levorotatory (-)-2-[2-[4-[(4-chlorophenyl)phenylmethyl]-1-piperazinyl]ethoxy]acetamide are obtained.

1. temperatureThe mixture is heated
2. temperatureat reflux temperature for 24 hours
3. filtrationthe mixture is filtered while hot through Dicalite
4. washThe filtrate is washed with 500 ml of water
5. customThe organic phase is separated
6. dry with materialdried over 250 g of sodium sulfate
7. filtrationIt is then filtered
8. custom10 the solvent is evaporated
9. temperatureThe solution is heated
10. temperatureunder reflux
11. customto crystallize
12. temperatureby cooling in an ice bath
13. filtrationThe crystals are filtered
14. washwashed with a small amount of diisopropyl oxide
15. customdried under vacuum at 40° C