反应详情

温度

23 °C

A solution of tert-butyl 2-(4-(3-(difluoro(quinolin-6-yl)methyl)-[1,2,4]triazolo[4,3-b]pyridazin-6-yl)phenyl)ethylcarbamate (70 mg, 136 mol) in DCM (1 mL) and TFA (1 mL) was stirred for 30 min at 23° C. The solvents were then removed under reduced pressure and crude product purified by RP-HPLC eluting with water/ACN (0.1% TFA). The desired collected fractions were then concentrated under reduced pressure and the resulting residue dissolved in MeOH/DCM (5 mL). Solution was then stirred as a suspension with Si-Carbonated (300 mg; 0.2 mmol) for 30 min at 23° C. The solids were then removed by filtration, washed with MeOH (3×1 mL), and filtrate concentrated under reduced pressure. The product was isolated as a white fluffy solid. MS (ESI pos. ion) m/z: 417 (MH+). Calc'd exact mass for C23H18F2N6: 416.

1. customThe solvents were then removed under reduced pressure and crude product
2. custompurified by RP-HPLC
3. washeluting with water/ACN (0.1% TFA)
4. customThe desired collected fractions
5. concentrationwere then concentrated under reduced pressure
6. dissolutionthe resulting residue dissolved in MeOH/DCM (5 mL)
7. customThe solids were then removed by filtration
8. washwashed with MeOH (3×1 mL), and filtrate
9. concentrationconcentrated under reduced pressure
10. customThe product was isolated as a white fluffy solid