PURPOSE: To obtain the subject compound useful as a raw material for optical materials having nonlinear optical effects, etc., or high strength and high elastic modulus molded bodes by oxidatively coupling an aromatic aminoacetylene compound in an organic solvent.

CONSTITUTION: A compound expressed by formula I (Ar is 6-12C bifunctional aromatic hydrocarbon group), e.g. m-aminophenylacetylene, is oxidatively coupled in an organic solvent using copper salts, manganese salts or cobalt salts as a catalyst and amines or an alkaline compound as a promoter at a temperature up to 100°C, preferably 20-80°C to afford a compound expressed by formula II, e.g. 1,4-di(3-aminophenyl)butadiyne. The catalyst is used in an amount of preferably 1-30% based on the compound expressed by formula I and the promoter is used in an amount of preferably 1mol based on 1mol catalyst.