丁香酸的制备新工艺

A New Process for Preparation of Syringic Acid

采用丁香醛为原料,经酯化、氧化、水解等反应步骤,制得丁香酸。本文研究了用量、温度和时间对制备丁香酸外观和纯度的影响,得出最佳制备工艺路线。路线分为三步:n(丁香醛)∶n(乙酸酐)=1.0∶2.5,回流条件下,制备丁香醛乙酰化产物;n(丁香醛)∶n(过氧化氢)=1.0∶2.0,60℃时制备丁香酸乙酰化产物;最后碱性/酸性水解丁香酸乙酰化产物,获得粗品含量>97%,产率>85%(n/n)的类白色丁香酸产品。

Syringic acid was prepared with syringa-aldehyde, using the esterification technique, oxidation technique and hydrolysis technique. Subsequently, the effects on the exterior and purity for this Syringic acid such as dosage, temperature and time were investigated. The optimum technological route of the synthetic of Syringic acid can be divided into three steps: First, the product of Syringaldehyde acetylation was prepared with syringa-aldehyde and acetic anhydride ( n ∶ n =1.0 ∶ 2.5) under the condition of reflux. Subsequently, the product of Eugenic acid acetylation was prepared by syringaldehyde and hydrogen peroxide ( n ∶ n =1.0 ∶ 2.0) at 60 ℃.Finally, Syringic acid with the crude content greater than 97% and yield more than 85% was obtained through subsequent the hydrolysis reaction of alkaline and acid.