Products of catalytic alkylation of PhOH with MeOH were analyzed by IR spectrometry and gas chromatog. to check the applicability of the methods for the process control. The mono, di and trimethylphenols as well as CO, CO2, CH4 and H2O were found in the products. No formation of PhOMe and p-MeC6H4OH was obsd. The IR spectrometry was recommended for monitoring the industrial process.