反应详情

温度

60 °C

5.000 g of 3-fluoro-5-[(2-fluoro-4-iodophenyl)amino]isonicotinic acid (13.294 mmol, 1. eq.) and 4.980 g of 1,1′-carbonyldiimidazol (30.710 mmol. 2.31 eq) were weighed into a round-bottom flask. 650 mL of dry DMF were added under a nitrogen atmosphere and the resulting mixture was stirred at 60° C. for 1.5 hours. The mixture was cooled to 3° C. in an ice bath, then ammonia (25 weight % in water) was added dropwise and the mixture stirred at room temperature for 18 hours. The resulting slurry was filtered off, the precipitate was rinsed with water and then dried in vacuo to yield 2.54 g (6.36 mmol, 48%) of the analytically pure target compound.

1. temperatureThe mixture was cooled to 3° C. in an ice bath
2. stirringthe mixture stirred at room temperature for 18 hours
3. filtrationThe resulting slurry was filtered off
4. washthe precipitate was rinsed with water
5. customdried in vacuo
6. customto yield 2.54 g (6.36 mmol, 48%) of the analytically pure target compound