Catalytic Cycloalumination for the Synthesis of Norbornane-Annulated Phospholanes

An effective one-pot method for the synthesis of polycyclic phospholanes by <i>in situ</i> reaction of dichlorophosphines (RPCl₂, where R = Ph, <i>t</i>-Bu, Me) with norbornane-annulated aluminacyclopentanes was obtained by catalytic cycloalumination of norbornenes. Oxidation of phospholanes gave the corresponding polycyclic phospholane 3-oxides (3-sulfides). The molybdenum complex L₂Mo­(CO)₄ (L = 3-phenyl-3-phosphatricyclo­[5.2.1.0^2,6]­decane) was prepared for the first time by the reaction of 3-phenyl-3-phosphatricyclo­[5.2.1.0^2,6]­decane with molybdenum hexacarbonyl. The structures of the obtained compounds were confirmed by X-ray diffraction and multinuclear ¹H, ¹³C, and ³¹P NMR spectroscopy