反应详情

A mixture of 1.67 g (0.005 mol) 1-(2-[bis(4-fluorophenyl)-methoxy]ethyl)piperazine, (U.S. Pat. No. 1545094), 1.89 g (0.010 mol) 3-chloropropyl-2-thienyl ketone, 1.52 g (0.011 mol) potassium carbonate and 30 ml methylisobutyl ketone was stirred and heated to reflux for 45 h. The reaction mixture was then evaporated in vacuo. The residue was redissolved in dichloromethane (1 00 ml) and washed twice with water (100 ml). The organic layer was then separated and dried with sodium sulfate. Evaporation in vacuo left a brown syrup. This was redissolved in dry ether and precipitated as the dihydrochloride with gaseous hydrogen chloride. The precipitate was collected by filtration and recrystallized from isopropanol. White crystals, m.p. 185°-88° C. (0.98 g=35%).

1. temperatureheated
2. temperatureto reflux for 45 h
3. customThe reaction mixture was then evaporated in vacuo
4. dissolutionThe residue was redissolved in dichloromethane (1 00 ml)
5. washwashed twice with water (100 ml)
6. customThe organic layer was then separated
7. dry with materialdried with sodium sulfate
8. customEvaporation in vacuo
9. waitleft a brown syrup
10. dissolutionThis was redissolved in dry ether
11. customprecipitated as the dihydrochloride with gaseous hydrogen chloride
12. filtrationThe precipitate was collected by filtration
13. customrecrystallized from isopropanol