二甲基姜黄素的合成工艺优化

Optimization of Synthesis Process of Dimethyl Curcumin

目的:对现有的二甲基姜黄素的合成路线进行工艺优化。方法:以乙酰丙酮作为起始原料,反应分两步进行,首先制得乙酰丙酮的硼络合物,然后与藜芦醛反应得到二甲基姜黄素,并对第二步的反应条件及后处理进行优化。结果:第二步反应制备二甲基姜黄素时,以N,N-二甲基乙酰胺(DMA)作为溶剂,反应温度为80℃,淬灭反应使用的酸用量为正丁胺的1.5当量,结晶补加水的体积为溶剂的2倍时,转化率最高。粗品收率95.1%,纯度98.6%,重结晶后总收率92.3%,纯度99.2%。结论:该路线原料廉价易得,反应条件温和,适合工业化生产。

Objective:To optimize the synthetic route of dimethyl curcumin.Method:Using acetylacetone as the starting material,the reaction was carried out in two steps.Firstly,the boron complex was prepared,and then reacted with veratrol to afford dimethyl curcumin.Then the reaction conditions and post-treatment were optimized.Results:In the second reaction step to prepare dimethyl curcumin,dimethylacetamide(DMA)was used as solvent,the reaction temperature was set at 80°C,the amount of acid used in quenching reaction was 1.5 equivalents to N-butylamine,and the volume of crystal water added was 2 times more than the volume of solvent.The conversion rate was very high.The crude yield was 95.1%,the purity was 98.6%,and the total yield after recrystallization was 92.3%,and the purity was 99.2%.Conclusion:The starting materials of this synthetic route are cheap and easy to obtain,and the reaction conditions are mild,and it is suitable for industrial production.