反应详情

温度

5 °C

4-[1-[3-(Isopropylamino)-2-pyridyl]piperazin-4-yl-carbonyl]benzoic acid (1.5 g) was dissolved in methylene chloride (50 ml) and then, triethylamine (0.7 ml) was added and cooled. Pivaloyl chloride (0.58 ml) was added slowly to the solution at 0~5° C. and the mixture was stirred at 5° C. for 2 hours. With the addition of piperazine (0.9 g), the solution was stirred at 5~10° C. for 3 hours. The reaction mixture was washed with water and aqueous sodium bicarbonate and the solvent was concentrated under reduced pressure. The concentrated residue was crystallized by treatment with ether and further recrystallized using isopropanol and ether. The recrystallized product was filtered and dried to give 1.48 g (yield: 83%) of the desired compound as white crystal.

1. temperaturecooled
2. stirringthe solution was stirred at 5~10° C. for 3 hours
3. washThe reaction mixture was washed with water and aqueous sodium bicarbonate
4. concentrationthe solvent was concentrated under reduced pressure
5. customThe concentrated residue was crystallized by treatment with ether
6. customfurther recrystallized
7. filtrationThe recrystallized product was filtered
8. customdried