依莰舒的合成工艺研究

Study on Synthetic Process of Ecamsule

探究了一种紫外线吸收剂依茨舒的合成优化工艺。以樟脑为原料,通过磺化、羟醛缩合和酸解反应合成依莰舒。采用核磁共振氢谱和红外光谱仪对其进行了结构表征,同时探究了原料配比、碱类型及用量、酸类型等对产品收率的影响。研究发现,合成依莰舒的最优条件为:投料摩尔比n对苯二甲醛∶n樟脑磺酸=1∶2.2,催化剂LDA的投入量为樟脑磺酸的1.8倍,酸解过程中选用强酸氢溴酸。最优条件下,依莰舒的收率为50.3%,纯度达到99.5%。

This paper discussed the synthetical technics of Escamsule with ultraviolet absorbent function.Using camphor as starting material,ecamsule was synthesized by sulfonation reaction,aldol condensation reaction and acid hydrolysis reaction.The structure of the target compound was characterized by NMR,MS and IR.At the same time,the effect on the yield of the target compound of the ratio of starting materials,the type and amount of alkali,and the type of acid was investigated.The results showed that the optimum conditions were as follows:molar ratio of terephthalaldehyde to camphorsulfonic acid was 1∶2.2,the type of alkali used as catalyst was Lithium diisopropylamide(LDA)with 1.8 times input amount more than camphorsulfonic acid.During acid hydrolysis,the acid was a strong acid hydrobromic acid.At the optimal reaction condition,the overall yield can reach 50.3%,and the purity can achieve 99.9%.