PURPOSE: To make possible the wide application of the titled compounds useful as liquid crystal materials, etc. and obtain the titled compounds by the easy synthetic method industrially and advantageously, by reacting an aryliminodimagnesium reagent which is a stable raw material with an aromatic nitro compound.

CONSTITUTION: An aryliminodimagnesium reagent of formula II (R2 is alkyl, alkoxyl, H, condensed aromatic ring or halogen; X is halogen) is reacted with an aromatic nitro compound of formulaI(R1 is alkyl, alkoxyl, OH condensed aromatic ring or halogen) to give an azoxyarene and azoarene. The azoxyarene is an asymmetric azoxyarene of formula III, asymmetric azoarene of formula IV and a symmetric azoarene of formula V. In case the compound of formula II is used in a molar amount of 1W2 times that of the compound of formulaI, the main product is the compound of formula III. In case the compound of formula II is used in a molar amount of 8W12 times, preferably 6W10 times, that of the compound of formulaI, the main product is the compound of formula IV.