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First examples of ene diamines with a phosphonate function at the C=C double bond were obtained by the reaction of dialkyl Hphosphonates with bis(N-tert-butyl)-diimine derived from glyoxal, [1,4-bis(tert-butyl)-1,4-diaza-1,3-butadiene], and isolated as hydrochlorides. Preferentially the cis-diamine is formed. The new phosphonates are characterized by multinuclear NMR spectroscopy( 1 H, 13 C, * Dr. A. Bogomilova Fax: +359-2-870-0309 E-Mail: anitabogomilova@abv.bg [a] Institute of Polymers 1213 31 P).In addition the methyl ester 8a was characterized by 14,15 N NMR spectroscopy as well as by several 2D NMR techniques and singlecrystal X-ray diffraction, unequivocally establishing the ene diamine structure. In the crystal dimers of the cations are formed by P-O···H-N hydrogen bonding.