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Optimization of the Ugi Reaction Using Parallel Synthesis and Automated Liquid Handling
Published on: November 11, 2008
Optimization of preparation conditions of medium and highly substituted carboxymethyl inulin through response surface
Dongkui Zhou1, Weichu Yu1, Aibin Wu1
1College of Chemistry & Environmental Engineering, Yangtze University, Jingzhou, 434023, Hubei, China.
Abstract:
This article introduces the synthesis optimization of carboxymethyl inulin using response surface methodology. The important factors affecting the degree of substitution (DS) were determined by Plackett-Burman design, including sodium hydroxide concentration, monochloroacetic concentration, and etherification temperature. Further optimization was conducted using the Box-Behnken response surface design. The coefficient of determination (R2) of the response surface model was 0.9827, and the adjusted R2 value was 0.9516, which proved the significance of the model. The optimized results of the predicted response showed that the molar ratios of sodium hydroxide to monochloroacetic acid and fructose to furan were 3.67 and 2.21, respectively. The maximum DS of 1.67 was obtained at 30 °C alkalization for 30 min and 50.30 °C etherification for 4 h, and the reaction efficiency (RE) reached 76.01 %. Under the optimized conditions, the Experimental DS was 1.68, suggesting that the experimental and predicted values of DS were in good agreement. The characterization results confirmed the synthesis of CMI. In this work, we have provided an effective method for the preparation of moderately to highly substituted CMI in 95 % ethanol.
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