Water → HCID 15480821, compound

Participants

Reaction Conditions

Reaction Steps

PHOSPHOROUS OXYCHLORIDE (2.8 ML, 30 MMOL) WAS ADDED TO A STIRRED MIXTURE OF 1-ETHOXYCARBONYLMETHYL-3-HYDROXY-6-METHYLPYRAZINONE (5.3 G, 25 MMOL) IN DRY TOLUENE (50 ML) UNDER ARGON. THE RESULTING MIXTURE WAS HEATED TO 60° C. AFTER 64 H, THE MIXTURE WAS COOLED AND WATER AND ETHYL ACETATE WERE ADDED. THE ORGANIC LAYER WAS DRIED (NA2SO4) AND EVAPORATED IN VACUO. THE RESIDUE WAS PURIFIED BY FLASH COLUMN CHROMATOGRAPHY ON SILICA GEL (50% ETOAC/HEXANES) TO GIVE THE TITLE COMPOUND AS A CRYSTALLINE SOLID:

Provenance & Evidence