Triethylamine → HCID 13393815, compound

Participants

Reaction Conditions

Reaction Steps

A solution of 25.7 g 4-chloro-3-hydroxyiminomethyl-flav-3-ene and 28.3 g triphenylphosphine in 250 ml 1,2-dichloroethane and 8.7 ml carbon tetrachloride is heated at 60° C. To this solution one adds 12.54 ml triethylamine. The temperature is maintained between 62°-65° C. during the addition and for further 25 minutes. The mixture is cooled to 0° C., filtered and evaporated. The crude material is extracted with hexane. The combined extracts are evaporated and purified by column chromatography on silicagel using a mixture of dichloromethane and hexane as eluant. The pure fraction is evaporated and crystallized in diisopropylether. Pure 4-chloro-3-cyano-flav-3-ene is obtained as pale yellow crystalls; m.p. 99° C.

Provenance & Evidence