NOWADAYS, THE PHOSPHORAMIDATES CHEMISTRY IS OF GREAT INTEREST DUE TO ITS WIDE APPLICATIONS IN VARIOUS AREAS OF SCIENCE SUCH AS MEDICINE [1], AGRICULTURE [2], COORDINATION CHEMISTRY [3], THEORETICAL CHEMISTRY AND STRUCTURAL [4] INVESTIGATIONS. THERE HAVE BEEN MANY EFFORTS FOR THE SYNTHESIS, CHARACTERIZATION AND STRUCTURAL INVESTIGATIONS ON THESE COMPOUNDS. IN THIS RESEARCH, FIRST ONE PHOSPHORAMIDE INTERMEDIATE 4-NO2C6H4NHP(O)CL2 WAS SYNTHESIZED. THEN, THE REACTION OF THISINTERMEDIATE WITH CH3OH AND ALLYLAMINE IN AN ULTRASONICBATH PRODUCED TWO NEW PHOSPHORAMIDESWITH FORMULA 4-NO2C6H4NHP (O) X2, WHERE X=OCH3 (1) AND NH-CH2-CH=CH2 (2). THE TWO NANOSIZEDCOMPOUNDS 1 AND 2 WERE CHARACTERIZED BY MULTINUCLEAR (1H, 13C, 31P NMR), FT-IR, FLUORESCENCESPECTRA, XRD PATTERNSAND FE-SEMANALYSES. THE 31P NMR SPECTRA REVEALED THE PHOSPHORUS CHEMICAL SHIFTS AT 3.59,3.48 AND 8.83,8.73 PPM FOR COMPOUNDS 1 AND 2, RESPECTIVELY. THE FT-IR SPECTRA SHOWED THE P=O STRETCHING FREQUENCIES FOR 1 AND 2 AT 1229, 1264 CM-1, RESPECTIVELY. THE FE-SEM IMAGES ILLUSTRATED THE SPHERICAL MORPHOLOGY OF THE NANOPARTICLES OF COMPOUNDS 1 AND 2 AS WELL AS THEIR AVERAGE PARTICLE SIZE OF  ~30-40 NM. THE XRD PATTERNS DISPLAYED SHARP PEAKS AT 14.58O (100%), 15.04O (83%), 17.85O (85%) AND 9.62O (100%), 17.71O (66%), 24.31O (57%) FOR PHOSPHORAMIDES1 AND 2, RESPECTIVELY. MOREOVER, THE PRESENCE OF SEVERAL SHARP PEAKS FOR BOTH COMPOUNDS VERIFIES THEIR HIGH CRYSTALLINITIES.