A new synthetic route for the preparation of aromatic 1,5‐diketones was developed through Ni(II)‐diphosphine‐catalyzed one‐pot reactions of various aromatic ketones with aromatic aldehydes in presence of KOH and 1,4‐dioxane in moderate yields. This protocol provides expeditious access to aromatic 1,5‐diones with a single step through cross‐aldol reaction followed by Michael 1,4‐addition and does not require expensive metal complexes as catalysts. All the synthesized catalysts and the products derived from the carbonyl compounds were fully characterized by spectroscopic and analytical data. The factors influencing the rate of reaction were discussed.
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