HCID 178472230, compound → HCID 178432187, compound

Participants

Reaction Conditions

Reaction Steps

To a suspension of ethyl 3-{[3-(7-fluoro-3-methylquinoxalin-2-yl)-1H-pyrazol-5-yl]amino}-3-oxopropanoate (30.0 g, 84.0 mmol) in methanol (210 mL), tetrahydrofuran (210 mL) and water (210 mL) was added 4-dimethylaminopyridine (51.3 g, 420 mmol) at ambient temperature. After being stirred at 85° C. for 5 h, the reaction mixture was diluted with ethyl acetate (750 mL) and water (750 mL) at ambient temperature. And the insoluble material was filtered off. The filtrate was washed with water (450 mL). The combined aqueous layer was washed with ethyl acetate (500 mL×2), and acidified to pH 2 with conc. Hydrochloric acid (17.0 mL) at ambient temperature, and then stirred for overnight. The resulting precipitate was collected and washed with water to give 2-(7-fluoro-3-methylquinoxalin-2-yl)pyrazolo[1,5-a]pyrimidine-5,7-diol. MS (APCI): m/z 312 (M+H).

Provenance & Evidence