草酸二龙脑酯的合成及其表征

Synthesis and Characterization of Dibornyl Oxalate

摘要:

在偏钛酸或者硼酐催化作用下，龙脑和草酸发生酯化反应生成草酸二龙脑酯，探讨了催化剂类型及用量、原料配比、反应温度以及反应时间对酯化反应的影响。结果表明，在50.0 g正己烷溶剂中，m(龙脑)∶m(草酸)∶m(催化剂)=5.0∶12.0∶3.0，于55 ℃下反应96 h时，龙脑的转化率及草酸二龙脑酯的选择性分别为95.8 %和99.4 %。通过HRMS、IR、1H NMR、13C NMR等对草酸二龙脑酯进行了鉴定与表征。

Abstract:

Dibornyl oxalate was synthesized from esterification reaction between borneol and oxalic acid catalyzed by metatitanic acid or boron anhydrous. The effect of reaction conditions such as selectivity and dosage of catalyst, material ratio, reaction temperature and reaction time on the conversion of borneol and product selectivity of dibornyl oxalate were explored. The results showed that the optimal synthetic conditions of this reaction were: mass ratio of borneol with anhydrous oxalic acid and catalyst 5.0∶12.0∶3.0, reaction temperature 55℃ and reaction time 96 h. Under the reaction conditions, the conversion rate of borneol and the selectivity of dibornyl oxalate were 95.8% and 99.4%, respectively. The structure of dibornyl oxalate was identified and characterized by HRMS, IR, 1H NMR and 13C NMR.