Partially substituted amylose n-butylcarbamate (ABC) samples were synthesized with weight-average molar mass M w ranging between 40 kg mol -1 and 220 kg mol -1 with different degree of substitution DS. When DS was between 0.17 and 0.33, the ABC samples were soluble in water. Furthermore, both LCST and UCST type phase separations were observed for the ABC samples in water when DS is >0.26. The closed-loop phase diagrams for the dual thermoresponsive ABC samples in water were constructed by turbidity measurement. The UCST ranged from 70 °C to 77 °C and the LCST ranged from 13 °C to 17 °C. SAXS measurements were performed for dilute aqueous ABC solutions to determine the chain conformation of ABC at various temperatures. The resulting form factor at the polymer mass concentration of 3 mg mL -1 indicated that the chain conformation is almost independent of temperature, except for the chain diameter, which is influenced by the temperature-dependent hydration behavior. This result suggests that the attractive interactions between ABC chains are not very significant even between UCST and LCST, where higher concentrated polymer solutions show macroscopic phase separation.