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A highly-efficient method for the copper- and solvent-free coupling reaction of acid chlorides and terminal alkynes catalyzed by diatomite-supported palladium(II) salophen complex is described. Acid chlorides are easily coupled with terminal alkynes, giving good to high yields in the presence of a low catalyst loading (1 mol% Pd) in DIEA at room temperature under aerobic conditions. After centrifugation, the supported catalyst is able to be recycled and reused for several times with only a slight decrease in activity.