反应详情

4-[1-[3-(Isopropylamino)-2-pyridyl]piperazin-4-yl-carbonyl]benzoic acid methyl ester (1.2 g) was dissolved in a co-solvent of ethanol (10 ml) and acetonitrile (20 ml), and 4-(2-aminoethyl)morpholine (0.82 g) was added. The reaction mixture was heated to reflux for 15 hours and cooled. After excess of water was added to the solution at 30° C. to precipitate the crystals, the solution was stirred for 1 hour. Then, the solution was again cooled slowly, stirred at 10~15° C. for 2 hours and filtered. The filtered crystal was washed with preheated water(40° C.) and was recrystallized using isopropanol and ether, filtered and dried to give 1.22 g (yield: 81%) of the desired compound.

1. additionwas added
2. temperatureThe reaction mixture was heated
3. temperatureto reflux for 15 hours
4. temperaturecooled
5. customto precipitate the crystals
6. temperatureThen, the solution was again cooled slowly
7. stirringstirred at 10~15° C. for 2 hours
8. filtrationfiltered
9. washThe filtered crystal was washed with preheated water(40° C.)
10. customwas recrystallized
11. filtrationfiltered
12. customdried