A rapid synthetic procedure for the preparation of phospholanium perchlorates in high yield has been developed. The process involves the cleavage of tetrahydrofuran by lithium organophosphides, affording 4-hydroxybutylorganophosphines, which are then intramolecularly cyclized in an aqueous solution. The following phospholanirim salts (very tediously prepared by other methods) have been obtained by this procedure: ...