反应详情

温度

60 °C

N-(4-((1-(4-methoxybenzyl)-1H-pyrazolo[3,4-b]pyridin-4-yl)(2-morpholinoethyl)amino)-3-fluorophenyl)-2-(4-fluorophenyl)-3-oxo-2,3-dihydropyridazine-4-carboxamide (0.015 g, 0.02165 mmol) was dissolved in TFA (0.1668 ml, 2.165 mmol) and stirred at 60° C. for 18 hours. Excess TFA was evaporated, and the crude product was then resuspended in toluene and reconcentrated to remove trace TFA. The crude solid was then partitioned between EtOAc and NaHCO3. The organic layer was separated and dried over sodium sulfate. After filtration to remove sodium sulfate and concentration, the residual crude solid was taken up in a small amount of DCM and treated with 2N HCl in ether. The suspension was evaporated to dryness to give 14 mg (95%) of product as a brown solid. LRMS (apci pos): 573.3 (M+H)+.

1. customExcess TFA was evaporated
2. customto remove trace TFA
3. customThe crude solid was then partitioned between EtOAc and NaHCO3
4. customThe organic layer was separated
5. dry with materialdried over sodium sulfate
6. filtrationAfter filtration
7. customto remove
8. concentrationsodium sulfate and concentration
9. additiontreated with 2N HCl in ether
10. customThe suspension was evaporated to dryness