This invention is directed to the production of 2,2' -methylenebis (3, 4, 6-trichlorophenol), commonly known as hexachlorophene, by reacting 1 mol of 2, 4, 5-trichlorophenol, 1 mol of 2, 4, 5-trichlorophenylsulfate and 1 mol of formaldehyde in a solvent solution in which the 2, 4, 5-trichlorophenylsulfate has been prepared in situ by reacting 2, 4, 5-trichlorophenol with sulfurtrioxide.