Synthesis, Characterization and Reactivity of a Base‐Stabilized Dialane(4) Supported by Double Layer Nitrogen–Phosphorus Ligands

Comprehensive Summary We synthesized a dialane(4) compound ( 2 ) stabilized by double‐layer N‐P ligands. Upon reduction with KC 8 , compound 2 demonstrates solvent‐dependent reactivity: in THF, it undergoes C—O bond cleavage to yield product [MeN(CH 2 CH 2 NPiPr 2 ) 2 Al(CH 2 ) 4 O] 2 K 2 ; whereas in a THF/toluene mixture, it results in the activation of the methyl C—H bond in toluene, forming product [MeN(CH 2 CH 2 NPiPr 2 ) 2 AlH] 2 K 2 . We propose that these reactions involve an “Al(I)” intermediate, which facilitates oxidative addition with either the C—O bond of THF or the C—H bond of toluene.