反应详情

温度

0 °C

To a suspension of tert-butyl[(1-{[6-({3-(aminocarbonyl)-5-[2,6-difluoro-4-(1-hydroxy-1-methylethyl)phenyl]-2-thienyl}amino)pyridin-2-yl]methyl}-1H-1,2,3-triazol-4-yl)methyl]carbamate (90 mg, 0.15 mmol) in EtOAc (7.0 mL) at ° C. was added 4 M HCl in dioxane (1.88 mL, 7.50 mmol). The reaction was stirred at 0° C. for 4 h. The yellow suspension was quenched with saturated NaHCO3 and extracted with 5:1 CH2Cl2:MeOH (2×). The combined organic layers were dried (MgSO4), filtered, and evaporated. The residue was purified by reverse phase HPLC (15-75% MeCN/water w/0.025% TFA). Product fractions were neutralized with saturated NaHCO3, extracted with 5:1 CH2Cl2:MeOH (2×), dried (MgSO4), filtered, and evaporated to give the title compound as a yellow solid.

1. customThe yellow suspension was quenched with saturated NaHCO3
2. extractionextracted with 5:1 CH2Cl2
3. dry with materialThe combined organic layers were dried (MgSO4)
4. filtrationfiltered
5. customevaporated
6. customThe residue was purified by reverse phase HPLC (15-75% MeCN/water w/0.025% TFA)
7. extractionextracted with 5:1 CH2Cl2
8. dry with materialMeOH (2×), dried (MgSO4)
9. filtrationfiltered
10. customevaporated