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We aimed to construct a method involving the photocatalytic oxidative dehydrogenation of formic acid (FA) to promote the acetone reductive hydrogenation of C–C coupling, where photo-electrons and photo-holes could be effectively used. The results showed that the conversion rates of acetone and FA in the g-C3N4 photocatalytic acetone–FA coupling reaction system were 88.74% and 60.82%, respectively. Further research showed that the Na+ concentration on the surface of the C3N4 photocatalyst was also positively correlated with pinacol selectivity. The g-C3N4 treated with 5 M NaOH showed a high pinacol selectivity of 60.87%, which was increased by 32.30%. [ABSTRACT FROM AUTHOR]