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Various catalysts were used in a systematical study of selective catechol methylation to 3-methylcatechol (I) in a fixed-bed reactor of 35-mm diam. and 16-cm length. Reaction products were analyzed by gas chromatog. with mass spectrometric detection. Alumina of high purity was a suitable catalyst after partial deactivation. The formation of polymethylated catechol was avoided over this catalyst at conversion rates of 20%. The selectivity for the unwanted byproduct 4-methylcatechol was