反应详情

温度

150 °C

To a mixture of 4-amino-5-{4-[(5-chloro-3H-imidazo[4,5-b]pyridin-2-yl)amino]phenyl}-N-(2,2,2-trifluoroethyl)pyrrolo[2,1-f][1,2,4]triazine-6-carboxamide (50 mg, 0.1 mmol), p-tolylboronic acid (27 mg, 0.2 mmol), potassium carbonate (82 mg, 0.6 mmol), in DMF was added 1,1′-bis(diphenylphosphino)ferrocinepalladium (II) chloride (7.3 mg, 0.01 mmol). The mixture was then degassed using nitrogen for 10 min, and then heated (150° C.) in a microwave for 15 min. After cooling to room temperature, the mixture was diluted with methanol and concentrated under reduced pressure. The residue purified by silica gel chromatography using a 1 to 8% methanol/dichloromethane as the eluant to afford the desired product (5.9 mg, 11%). 1H-NMR (300 MHz, CD3OD) 7.86 (s, 1H), 7.81-7.87 (m, 4H), 7.73-7.79 (m, 2H), 7.63-7.69 (m, 1H), 7.53 (s, 1H), 7.40-7.49 (m, 2H), 7.22-7.28 (m, 2H), 3.92-3.99 (m, 2H), 2.38 (s, 3H); ES-MS m/z 558.3 (MH)+; HPLC RT (Method A) 2.64 min.

1. customThe mixture was then degassed
2. customfor 10 min
3. temperatureAfter cooling to room temperature
4. additionthe mixture was diluted with methanol
5. concentrationconcentrated under reduced pressure
6. customThe residue purified by silica gel chromatography