Hydrochloric Acid → HCID 86279105, compound

Participants

Reaction Steps

The compound from Preparation 18 (R)-tert-Butyl 3-(N-(3-chloropyridin-2-yl)-4-(5-(ethoxycarbonyl)-1-methyl-1H-pyrazol-4-yl)benzamido)piperidine-1-carboxylate (145.87 g, 256.8 mmol) was dissolved in 1.4 L of DCM and then treated with hydrochloric acid (3 mol/L in cyclopentyl methyl ether, 428 mL, 1284 mmol). The reaction was stirred at room temperature for 19 h then 500 mL of DCM was added followed by warming to 40° C. and then filtering through Celite®. The filtrate was concentrated to 500 mL total volume in vacuo and then added to 1.4 L of EtOAc, resulting in precipitation of solids which were isolated via filtration. After drying, the hydrochloride salt of the title compound was isolated as an off-white solid (125.2 g, 97%).

Provenance & Evidence