HCID 86747151, compound → HCID 178459029, compound

Participants

Reaction Steps

To 220 ml of acetic acid was added 22 g of 3-allyloxy-2-(α-hydroxyiminoisocaproylamino)propionitrile. The mixture was subjected to a reaction for 1 hour at 85° C. After completion of the reaction, acetic acid was removed by evaporation under reduced pressure. The residue was purified by using Frorisil (60-100 mesh) (eluting solvent: 30 volume % ethyl acetate-n-hexane→ 60% volume of ethyl acetate-n-hexane), then washed with diethyl ether, followed by recrystallization from benzene, to obtain 5 g of 6-allyloxymethyl-5-amino-3-isobutyl-1,2-dihydropyrazin-2-one 4-oxide (Compound B-3) as pale yellow plate-like crystals having a melting point of 149°-151° C.

Provenance & Evidence