乙酰阿魏酰氯合成工艺的优化

Optimum synthesis of acetylferuloyl chloride by orthogonal design

目的优化乙酰阿魏酰氯的合成工艺。方法先以香草醛和乙酸酐等为原料,经Perkin反应合成乙酰阿魏酸,进一步制备乙酰阿魏酰氯。按正交表L9(34)表设计考察乙酰阿魏酸和乙酰阿魏酰氯合成的影响因素,对乙酰阿魏酸合成中反应时间、PEG-400用量及投料比等因素进行优选,同时也考察乙酰阿魏酰氯合成的反应时间、反应温度及乙酰阿魏酸与氯化亚砜的摩尔比等因素对吸收率的影响。结果前者最佳工艺为A1B2C1,后者最佳工艺为A1B2C2,两步总收率达65%。结论该最佳工艺可缩短反应时间,提高生产效率,适合工业生产。

Objective To optimise the process of acetylferuloyl chloride. Methods Using vanillin and acetic anhydride ere as raw materials, to synthesize acetyl-ferulic acid through Perkin reaction, finally acetylferuloyl chloride was synthesized. The main factors influenced yield of synthesis acetylferuloyl chloride and acetylferulic acid were evaluated,within synthesis acetylferuloyl chloride such as reaction time,reaction temperature and ratio of acetyl-ferulic acid and SOCl2 and within synthesis acetylferulic acid such as reaction time, the quantity of PEG-400 and material-ratio,by the orthogonal experimental design of L9 （3^4 ） orthogonal design. Results The optimization terms of the process of the former were A1 B2 C1 , and the latter were A1 B2 C2 , the total yield reached 65%. Conclusion The best process could improve efficiency,shorten the reaction time,the experimental method was suitable for industrial production of acetylferuloyl chloride.