PURPOSE: To prepare the titled compound useful as a raw material of pharmaceuticals and agricultural chemicals, easily, in high yield, by reacting 4-nitrophenetol with formaldehyde and hydrochloric acid in the presence of concentrated sulfuric acid and an electrophilic metallic chloride.

CONSTITUTION: 2-Chloromethyl-4-nitrophenetol is prepared by reacting 4-nitrophenetol with formaldehyde compound (e.g. formalin, paraformaldehyde, etc.) in the presence of concentrated sulfuric acid and an electrophilic metallic chloride such as zinc chloride, ferric chloride, cupric chloride, etc. The amount of formaldehyde is more than equivalent based on 4-nitrophenetol, and that of zinc chloride, etc. is usually 0.001W1 equivalent. When a compound such as NaCl, KCl, etc. is used in combination with the electrophilic metallic chloride, the load for the treatment of heavy metal in the waste water can be reduced.