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A one-step procedure to obtain modified fibers containing n-decyl phosphate cellulose is proposed. The reaction was carried out at 150 °C in heterogeneous conditions with kraft pulp fibers in the presence of n-decyl monophosphate and N,N-dimethylacetamide (DMAc). The simultaneous addition of phosphorus and alkyl chain was characterized by solid-state nuclear magnetic resonance (13C and 31P-NMR), Fourier transform infrared spectroscopy and energy dispersive X-ray spectroscopy. The phosphorus content, estimated at 2.0%, was determined by UV-visible spectrophotometry. Results also indicated that grafted phosphate groups wear alkyl chains.