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5-bromo-2,3-dimethoxy-6-methyl-1,4-benzoquinone 3, a key intermediate for preparing coenzyme Q compounds, was readily synthesized in two steps by a reaction sequence starting from the commercially available 3,4,5-trimethoxytoluene 1 via bromination and oxidation reactions. Persulfate salts were first employed as oxidants to synthesize 1,4-benzoquinone, the overall yield of title compound 3 was 65%.