反应详情

温度

70 °C

N-(2-(2,5-Difluorophenyl)-5-methylpyridin-4-yl)-1-(4-methoxybenzyl)-1H-pyrazolo[4,3-b]pyridin-7-amine and N-(2-(2,5-difluorophenyl)-5-methylpyridin-4-yl)-2-(4-methoxybenzyl)-2H-pyrazolo[4,3-b]pyridin-7-amine and trifluoroacetic acid (35.0 mL) were combined and heated at 70° C. for 3 hours. The reaction was then cooled and concentrated to give a residue which was dissolved in dichloromethane (75 mL) and added with stirring to a saturated sodium bicarbonate solution (50 mL) to give a solid. The solid was collected by filtration and dissolved in ethyl acetate (500 mL) which was extracted with brine (50 mL), dried over magnesium sulfate, filtered, and concentrated to give title compound. 1H NMR (400 MHz, DMSO-d6) δ ppm 2.37 (3H, s) 7.09 (1H, d, J=4.80 Hz) 7.26-7.36 (2H, m) 7.50 (1H, s) 7.75 (1H, ddd, J=9.54, 6.13, 3.28 Hz) 8.24 (1H, d, J=1.26 Hz) 8.35 (1H, d, J=5.05 Hz) 8.43 (1H, s) 8.50 (1H, s) 13.03 (1H, s). MS [M+H] found 338.3.

1. temperatureThe reaction was then cooled
2. concentrationconcentrated
3. customto give a residue which
4. additionadded
5. customto give a solid
6. filtrationThe solid was collected by filtration
7. dissolutiondissolved in ethyl acetate (500 mL) which
8. extractionwas extracted with brine (50 mL)
9. dry with materialdried over magnesium sulfate
10. filtrationfiltered
11. concentrationconcentrated