柠康酸酐的合成研究

Synthesis of citraconic anhydride

研究了衣康酸催化脱水合成柠康酸酐,考察了催化剂种类和用量、带水剂种类和用量、反应时间等因素对反应结果的影响,得到了最佳反应条件,即衣康酸15g,溶剂二甲苯15g,催化剂硫酸镁0.175g,反应时间6h。在上述条件下,柠康酸酐收率和质量分数分别为83.1%和97.9%。此外,采用1 H NMR、13 C NMR和FT-IR等技术手段表征了所得产品,结果表明,所得产品即为目标化合物。

The synthesis of citraconic anhydride in the presence of catalyst was studied in this pa- per. The effects of factors, such as kind and dosage of catalyst, kind and dosage of solvent, and reaction time,were examined. The optimum conditions were obtained as follows： Itaconic acid 15 g,water carry- ing agent dimethylbenzene 15 g,catalyst magnesium sulphate 0. 175 g, reaction time 6.0 h. Under the above reaction conditions, the yield and the purity of citraconic anhydride were more than 83% and 97.9% ,respectively. The structure of the product was characterized by the 1H NMR,13C NMR and FT-IR. And the results showed that the synthesized product was the target compound.