反应详情

温度

5 °C

Triethylamine (0.54 ml) was added to 6-[1-[3-(isopropylamino)-2-pyridyl]piperazine-4-yl-carbonyl]nicotinic acid (1.3 g) in methylene chloride (40 ml) for dissolution and cooled. With the slow addition of pivaloyl chloride (0.45 ml) at 0° C.˜5° C., the reaction mixture was stirred at 5° C. for 2 hours. With the addition of triethylamine (0.6 ml) and ethanolamine (0.25 ml), the mixture was stirred at 5° C.˜10° C. for 3 hours. The solution was washed with aqueous sodium bicarbonate and water twice. The separated organic layer was concentrated under reduced pressure. The concentrated residue was treated with ether for crystallization and recrystallized with ethanol and isopropyl ether to give a desired compound of 1.2 g (yield: 83%).

1. temperaturecooled
2. stirringthe mixture was stirred at 5° C.˜10° C. for 3 hours
3. washThe solution was washed with aqueous sodium bicarbonate and water twice
4. concentrationThe separated organic layer was concentrated under reduced pressure
5. additionThe concentrated residue was treated with ether for crystallization
6. customrecrystallized with ethanol and isopropyl ether