Hydrochloric Acid → HCID 118389985, compound

Participants

Reaction Steps

To a suspension of tert-butyl 9-((5-chloro-2-((1-methyl-1H-pyrazol-4-yl)amino)pyrimidin-4-yl)(methyl)amino)-3-azaspiro[5.5]undecane-3-carboxylate (330 mg, 0.67 mmol) in dichloromethane (15 mL) was added the solution of HCl in EtOAc (3 mL, 12 mmol). The reaction mixture was stirred at rt for 2 h and then adjust to pH=8-9 with the solution of saturated NaHCO3. The resulting mixture was diluted with 20 mL of H2O and exacted with a mixture of DCM and MeOH (10/1, 10 mL×3). The combine organic layers were washed with brine (20 mL×1), then over Na2SO4, filtered and concentrated in vacuo. The residue was purified by flash silica gel column chromatography (DCM/MeOH (v/v)=10/1 to 5/1) to give the title compound as a yellow solid (170 mg, 64.8%).

Provenance & Evidence