反应详情

温度

5 °C

Triethylamine (0. 8 ml) was added to 6-[1-[3-(isopropylamino)-2-pyridyl]piperazin-4-yl-carbonyl]nicotinic acid (2g) in methylene chloride (30 ml) for dissolution and cooled. With the slow addition of pivaloyl chloride (0. 7 ml) at 0° C.˜5° C., the mixture was stirred at 5° C for 1 hour. With the successive addition of triethylamine (0.9 ml) and 2-thiophenethylamine (0.75 g), the mixture was stirred at 5° C.˜10° C. for 2 hours. The solution was washed with an aqueous sodium bicarbonate and water. The separated organic layer was dried over magnesium sulfate and concentrated under reduced pressure. The concentrated residue was treated with ether for crystallization. The solid, so obtained, was recrystallized with ethanol and hexane to give a desired compound of 1.92 g (yield: 74%).

1. temperaturecooled
2. stirringthe mixture was stirred at 5° C.˜10° C. for 2 hours
3. washThe solution was washed with an aqueous sodium bicarbonate and water
4. dry with materialThe separated organic layer was dried over magnesium sulfate
5. concentrationconcentrated under reduced pressure
6. additionThe concentrated residue was treated with ether for crystallization
7. customThe solid, so obtained
8. customwas recrystallized with ethanol and hexane