The addition of AlCl3, to a dichloromethane solution of a triphosphenium tetrachloroaluminate R3P-P-PR3 AICI4 leads to chloromethylation of the latter, and in a subsequent reaction to the formation of 1,2-diphosphonio-diphosphirane tetrachloroalum inates. It is essential for this second step, that at least one R3P group of the two triphosphenium ions entering the reaction is aminosubstituted. The structure o f the diphosphonio-diphosphirane ions is established by NMR spectroscopy and in one case by X-ray investigation
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