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Cobalt(II) chloride hexahydrate (CoCl 2 ⋅6H 2 O) has been found to be an efficient catalyst for the one-pot synthesis of biscoumarin derivatives through a combination of aromatic aldehydes and 4-hydroxycoumarin in aqueous media at 70 ∘ C. Several types of aromatic aldehyde, containing electron-withdrawing groups as well as electron-donating groups, were used in the reaction and in all cases the desired products were synthesized successfully. The present approach offers remarkable advantages such as short reaction times, excellent yields, straightforward procedure, easy purification, environment friendliness, and low catalyst loading.