N',N'-disubstituted N-diphenoxyphosphorylureas, (PhO)2P(O)-NH-CO-NR1R2 (R1 = R2 = Et, 1; n-Pr, 2; n-Bu, 3; i-Bu, 4; R1 = Me and R2 = Ph, 5) as well as phosphorylated biuret compounds, (PhO)2P(O)-NH-CO-NH-CO-NR1R2 are obtained in the reaction of diphenoxyphosphorycholride with N,N-disubstituted ureas and triethylamine. The biuret derivatives are formed via (PhO)2P(O)NCO. Theiry ield rises if the reaction is carried out without amine. The X-ray crystal structure analysis of (PhO)2P(O)-NH-CO-NH-CO-NPr2, 8, shows that dimers exist in the crystal with intermolecular as well as intramolecular hydrogen bonds. The framework formed by atoms P-N1-C1(O4)-N2-C2(O5)-N3(C3)C6 is planar. The existence of a rotation barrier along the bond C2-N3 was detected by NMR spectroscopy.