A number of phenols and hydroxyheterocyclic compounds have been converted to the corresponding thiol compounds by the route, phenol to 0-aryl dialkylthiocarbamate to S-aryl dialkylthiocarbamate to thiophenol. Methods for accomplishing each step in high yield are described. Since the thiol compounds formed are readily desulfurized by heating with Raney nickel, a useful way of replacing aromatic hydroxyl groups by hydrogen is at hand.