反应详情

温度

-10 °C

A 1.52 g portion of 4-hydroxyphthalonitrile was dissolved in 30.0 ml of acetonitrile, mixed with 2.1 ml of triethylamine and stirred at −10° C. The reaction solution was mixed with 1.8 ml of anhydrous trifluoromethanesulfonic acid, stirred at 0° C. for 30 minutes and then warmed up to room temperature, mixed with 15 ml of DMF and stirred for 2 hours. After evaporation of the solvent under reduced pressure, the residue was mixed with ethyl acetate and washed with saturated aqueous sodium bicarbonate and then the organic layer was dried over sodium sulfate. After evaporation of the solvent under reduced pressure, the residue was dissolved in 20 ml of acetonitrile and mixed with 2.30 g of 2,5-transmethylpiperazine, and the mixture was heated under reflux for 2 hours and then stirred overnight at room temperature. After evaporation of the solvent under reduced pressure, the residue was mixed with 100 ml of ethyl acetate, washed with saturated aqueous sodium bicarbonate and saturated brine and then dried over sodium sulfate. The title compound was obtained by evaporating the solvent under reduced pressure.

1. stirringstirred at 0° C. for 30 minutes
2. temperaturewarmed up to room temperature
3. stirringstirred for 2 hours
4. customAfter evaporation of the solvent under reduced pressure
5. additionthe residue was mixed with ethyl acetate
6. washwashed with saturated aqueous sodium bicarbonate
7. dry with materialthe organic layer was dried over sodium sulfate
8. customAfter evaporation of the solvent under reduced pressure
9. dissolutionthe residue was dissolved in 20 ml of acetonitrile
10. additionmixed with 2.30 g of 2,5-transmethylpiperazine
11. temperaturethe mixture was heated
12. temperatureunder reflux for 2 hours
13. stirringstirred overnight at room temperature
14. customAfter evaporation of the solvent under reduced pressure
15. additionthe residue was mixed with 100 ml of ethyl acetate
16. washwashed with saturated aqueous sodium bicarbonate and saturated brine
17. dry with materialdried over sodium sulfate