Four kinds of new compounds,1,4-bis(chloromethy1)-2-methoxy-5-ethoxy benzene,1,4-bis(chloromethy1)-2-methoxy-5-butoxybenzene,1,4-bis(chloromethyl)-2-methoxy-5-heptyloxybenzene and 1,4-bis(chloromethy1)-2-methoxy-5-octyloxybenzene, are synthesized by using the chloromethylation of respective 1-methoxy-4-alkoxybenzene. The structure of these compounds is characterized by IR and ¹HNMR.