反应详情

温度

70 °C

To a vial containing N-(2-(5-chloro-2-fluorophenyl)pyridin-4-yl)-2-(4-methoxybenzyl)-2H-pyrazolo[4,3-b]pyridin-7-amine was added 5 mL of neat TFA and the mixture was heated at 70° C. for 3 hours. Cooled to room temperature and concentrated to dryness. The residue was purified by preparative HPLC eluting with a gradient of 10-30% acetonitrile (containing 0.035% TFA) in water (containing 0.05% TFA) using a Sunfire Prep 5 μm C18, 75×30 mm column conditions to give, after drying in vacuo, the title compound as a TFA salt as an off-white solid. 1HNMR (400 MHz, DMSO-d6) δ ppm 7.31-7.60 (4H, m) 7.62 (1H, ddd, J=8.78, 4.11, 2.78 Hz) 7.86 (1H, br. s.) 8.01 (1H, dd, J=6.69, 2.65 Hz) 8.56 (2H, d, J=6.32 Hz) 8.75 (1H, d, J=5.81 Hz) 11.12 (1H, br. s.), MS [M+H] found 340.2.

1. temperatureCooled to room temperature
2. concentrationconcentrated to dryness
3. customThe residue was purified by preparative HPLC
4. washeluting with a gradient of 10-30% acetonitrile (containing 0.035% TFA) in water (containing 0.05% TFA)
5. customto give
6. customafter drying in vacuo