HCID 86747152, compound → HCID 178470403, compound

Participants

Reaction Steps

400 Milliliters of acetic acid was added to 35 g of ethyl 2-cyano-2-(α-hydroxyiminoisocaproylamino)acetate. The mixture was subjected to a reaction for 1 hour at 70° C. Acetic acid was removed by evaporation, then the residue was mixed with toluene, and toluene was removed by evaporation. This procedure was repeated several times. The residue was purified by a silica gel column chromatography (eluting solvent: 50% by volume of ethyl acetate-n-hexane), followed by recrystallization from ethanol to obtain 21.3 g of 5-amino-6-ethoxycarbonyl-3-isobutyl-1,2-dihydropyrazin-2-one 4-oxide (Compound B-9) as yellow needle-like crystals having a melting point of 179°-181° C.

Provenance & Evidence