A convenient strategy has been developed for the preparation of various phosphine ligands in good to excellent yields through a nickel‐catalyzed C–P bond‐forming step. This reaction proceeded smoothly and tolerated a variety of functional groups to provide a new method for the synthesis of important phosphine ligands through the direct cleavage of a C–Cl bond.

An efficient strategy for the regioselective ortho-acylation of azoxybenzenes with various aldehydes in the presence of palladium catalysts has been developed and furnishes good to excellent yields. The reaction proceeds smoothly and can tolerate a variety of functional groups.

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