Hydrochloric Acid → HCID 118390008, compound

Participants

Reaction Steps

To a suspension of tert-butyl 8-((5-chloro-2-((1-methyl-1H-pyrazol-4-yl)amino)pyrimidin-4-yl)(methyl)amino)-2-azaspiro[4.5]decane-2-carboxylate (3.9 A: 0.15 g, 0.32 mmol) in DCM (10 mL) was added a solution of HCl in EtOAc (10 mL, 3.5 M). The mixture was stirred at room temperature for 2 h, then concentrated in vacuo. The residue was diluted with DCM (20 mL) and saturated Na2CO3 solution (20 mL). The organic layer was separated and the aqueous layer was extracted with a mixture of DCM and MeOH (10/1 (v/v), 20 mL×5). The combined organic layers was washed with brine (30 mL), dried over anhydrous Na2SO4, then filtered and concentrated in vacuo. The residue was purified by silica gel column chromatography (DCM/2N NH3 in MeOH (v/v)=5/1) to afford 3.10 A as a brown solid (0.10 g, 84%).

Provenance & Evidence