The substitution reactions of hexachlorocyclotriphosphazene, N3P3Cl6 (I), With 2-allylphenol to synthesize the partially substituted (2-allylphenoxy) chlorocyclotriphosphazenes, N3P3Cl6-i(OC6H4CH2CHCH2)(i), i = 1 similar to 6 by phase-transfer catalysis in an organic phase/alkaline solution were investigated. The reaction system was controlled by both chemical kinetics and mass transfer. The chemical shifts and coupling constants were proportional to the degree of substitution. The activation energy was predicted by the linear relationship between activation energy difference and P-31 chemical shift. In addition, the corresponding energies, enthalpies, and entropies of activation of the series substitution were also estimated.