Abstract: | A practical protocol for the decarbonylation of a wide range of aldehydes has been developed by using commercially available RhCl3⋅3 H2O and dppp in a diglyme solution. This method gives rise to decarbonylated products in good to high yield and is particularly useful because of its experimental simplicity, high generality and excellent level of functional group tolerance. The reaction has been applied in a tandem Oppenauer oxidation‐decarbonylation sequence, which removes a hydroxymethyl group in one operation. |