反应详情

温度

50 °C

A solution of N-(4-(1-(4-methoxybenzyl)-3-(1-methylpiperidin-4-ylamino)-1H-pyrazolo[3,4-b]pyridin-4-yloxy)-2-chloro-5-fluorophenyl)-2-(4-fluorophenyl)-3-oxo-2,3-dihydropyridazine-4-carboxamide (100 mg, 0.138 mmol) was dissolved in TFA (2 mL) and the solution was heated to 50° C. for 1 hour. Excess TFA was evaporated and the crude material was dissolved in EtOAc. The organic layer washed with saturated aqueous NaHCO3, brine, dried with Na2SO4, filtered and concentrated to afford a yellow solid. The solid washed with diethyl ether to afford the product (35 mg, 41.9% yield) as a yellow solid. LRMS (APCI pos) m/e 607.0 (M+H). 1H NMR (DMSO-d6, 400 MHz) δ 12.32 (s, 1H), 12.22 (s, 1H), 8.70 (d, 1H), 8.42 (dd, 12H), 8.17 (d, 1H), 7.91 (d, 1H), 7.74-7.67 (m, 2H), 7.49-7.41 (m, 2H), 6.17-6.13 (m, 1H), 5.23-5.18 (m, 1H), 3.60-3.42 (m, 1H), 2.85-2.73 (m, 2H), 2.20 (s, 3H), 2.10-1.96 (m, 4H), 1.65-1.53 (m, 2H).

1. customExcess TFA was evaporated
2. dissolutionthe crude material was dissolved in EtOAc
3. washThe organic layer washed with saturated aqueous NaHCO3, brine
4. dry with materialdried with Na2SO4
5. filtrationfiltered
6. concentrationconcentrated
7. customto afford a yellow solid
8. washThe solid washed with diethyl ether