反应详情

温度

0 °C

1-(1-(4-pyridyl)piperdin-4-ylcarbonyl)piperazine (0.411 g) was dissolved in dry dichloromethane (20 mL) and stirred under argon at 0° C. To the resulting solution was added triethylamine (0.56 mL) followed by the dropwise addition of a solution of 4-cyanobenzenesulphonyl chloride (0.33 g, 1.6 mmol) in dry pyridine (20 mL). The reaction was then stirred at 0° C. for 10 minutes and then allowed to warm to room temperature and stirred for a further 1 hour. The reaction was quenched by the removal of the dichloromethane and pyridine solvents by evaporation, taken up in water (60 mL) and then extracted with ethyl acetate (3×50 mL). The organic extracts were then washed with water, brine, dried (MgSO4) and evaporated to dryness. The product was then recrystallised to give 1-(4-cyanophenylsulphonyl)-4-(1-(4-pyridyl)piperidin-4-ylcarbonyl)piperazine as a white, hygroscopic solid m.p. 168-169° C.;

1. stirringThe reaction was then stirred at 0° C. for 10 minutes
2. temperatureto warm to room temperature
3. stirringstirred for a further 1 hour
4. customThe reaction was quenched by the removal of the dichloromethane and pyridine solvents by evaporation
5. extractionextracted with ethyl acetate (3×50 mL)
6. washThe organic extracts were then washed with water, brine
7. dry with materialdried (MgSO4)
8. customevaporated to dryness
9. customThe product was then recrystallised