反应详情

tert-Butyl 4-(2-([1,2,4]triazolo[4,3-a]pyridin-3-yl)-6-fluoroquinolin-8-yloxy)-3,3-difluoropiperidine-1-carboxylate (0.072 g, 0.144 mmol) was dissolved in MeOH (0.72 mL) and treated with 4.0 M HCl in dioxane (0.360 mL, 1.44 mmol), then stirred at ambient temperature for 2 hours. The reaction mixture was concentrated in vacuo. The residue was taken up in MeOH and concentrated three times. The residue was chromatographed on SiO2 eluting with a gradient of 2% NH4OH in isopropanol/methylene chloride. The desired product was dissolved in MeOH (2 mL), treated with 2.0 M HCl in ether (0.809 mL, 1.62 mmol) and concentrated in vacuo. The residue was again dissolve in MeOH and concentrated in vacuo several times, then placed under vacuum to give the desired product as a white solid (27.8 mg). MS APCI (+) m/z 400.3 (M+1) detected.

1. concentrationThe reaction mixture was concentrated in vacuo
2. concentrationconcentrated three times
3. customThe residue was chromatographed on SiO2 eluting with a gradient of 2% NH4OH in isopropanol/methylene chloride
4. dissolutionThe desired product was dissolved in MeOH (2 mL)
5. concentrationconcentrated in vacuo
6. dissolutionThe residue was again dissolve in MeOH
7. concentrationconcentrated in vacuo several times