Summary: 3‐Mono‐O‐(2‐methoxyethyl) cellulose (MEC) was selectively oxidized with 2,2,6,6‐tetramethyl‐1‐piperidinyloxy radical (TEMPO)/NaBr/ NaOCl. According to 1D and 2D NMR measurements, the primary hydroxyl group was completely oxidized without affecting the secondary one at position 2. Size‐exclusion chromatography revealed high tendency of 3‐mono‐O‐(2‐methoxyethyl)‐6‐carboxyl cellulose (MECO) to aggregate. Viscosity measurement and gelation of MECO upon interaction with chitosan and Cu2+ ions confirmed the introduction of anionic ions into the polymer backbone. Both MEC and MECO expressed the property of surface activity hence decreasing the surface tension of water (72 mN/m), being 45.0 and 56.8 mN/m, respectively.
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