反应详情

To a solution of tert-butyl 9-((5-chloro-2-((1-(2-hydroxyethyl)-1H-pyrazol-4-yl)amino) pyrimidin-4-yl)amino)-3-azaspiro[5.5]undecane-3-carboxylate (500 mg, 0.99 mmol) in dichloromethane (20 mL) was added a solution of HCl in EtOAc (5 mL, 20 mmol). The mixture was stirred at room temperature for 2 h and then concentrated in vacuo. The residue was dissolved in methanol (2 mL) and adjust to pH=7-8 with the solution of NaHCO3 and extracted with DCM (100 mL×3) The combined organic phases were washed with brine (100 mL), dried over anhydrous Na2SO4, filtered and concentrated in vacuo. The residue was purified with a silica gel column chromatography (MeOH/DCM (v/v)=1/10 to 1/7) to give the product as a light yellow solid (340 mg, 84.77%).

1. concentrationconcentrated in vacuo
2. dissolutionThe residue was dissolved in methanol (2 mL)
3. extractionextracted with DCM (100 mL×3) The combined organic phases
4. washwere washed with brine (100 mL)
5. dry with materialdried over anhydrous Na2SO4
6. filtrationfiltered
7. concentrationconcentrated in vacuo
8. customThe residue was purified with a silica gel column chromatography (MeOH/DCM (v/v)=1/10 to 1/7)