4-methyl-2-hydroxythiophenol(A) was synthesized by nitration, reduction and diazotization of p-thiophenol. The influence of dosage of NaNO2, concentration of sulfuric acid, temperature and concentration of H2SO4 in hydrolysis reaction on the yield of 4-methyl-2-hydroxythiophenol was studied. A high yield (71.2%) was achieved under the optimal reaction conditions. And a new chelating resin (B) containing o-hydroxythiophenol was synthesized through chlorosulfonation, reduction and the optimal reactions above. The FT-IR was used to identify the formation of 4-methyl-2-hydroxythiophenol and chelat...