Hydrogen chloride-ethyl acetate → HCID 131729107, compound

Participants

Reaction Steps

To (S)—N-(1-tert-butoxycarbonyl-pyrrolidin-2-ylmethyl)-4,6-dichloro-N-[3-(4-methyl-5-oxo-4,5-dihydro-1,3,4-oxadiazol-2-yl)phenyl]-2-methylthiopyrimidine-5-carboxamide (1.30 g, 2.18 mmol) obtained in Step 6 was added 4 mol/L hydrochloric acid-ethyl acetate (11 mL), and the mixture was stirred at room temperature for 1 hour. The mixture was concentrated under reduced pressure, and the residue was crystallized from hexane and ethyl acetate. The resulting solid was filtered and dried. This procedure was repeated to give (S)-4,6-dichloro-N-(pyrrolidin-2-ylmethyl)-N-[3-(4-methyl-5-oxo-4,5-dihydro-1,3,4-oxadiazol-2-yl)phenyl]-2-methylthiopyrimidine-5-carboxamidehydrochloride (898 mg, 77%).

Provenance & Evidence