草酸二异龙脑酯的合成及其结构表征

Synthesis and Structural Characterization of Diisobornyl Oxalate

通过莰烯和草酸在硼酐催化作用下的重排加成(酯化)反应合成了草酸二异龙脑酯,探讨了原料配比、催化剂用量、反应温度以及反应时间对酯化反应的影响。研究结果表明,莰烯(13.6 g)、草酸和催化剂的质量比为1.7∶2∶1,反应温度为55℃、反应时间为96 h的条件下,莰烯的转化率为89.5%,草酸二异龙脑酯的选择性为95.6%。产物通过IR、LCMS-IT-TOF、1H NMR、13C NMR等手段进行了结构鉴定与表征。

Diisobornyl oxalate was obtained by rearrangement,addition and esterification reactions from camphene and oxalic acid with boric anhydride as catalyst. The effects of reaction conditions such as material ratio,dosage of catalyst,reaction temperature and reaction time on the conversion of camphene and the selectivity of diisobornyl oxalate were explored. The results showed that the optimal synthetic conditions were： the mass ratio of camphene,anhydrous oxalic acid and catalyst 1. 7 ∶ 2 ∶ 1,reaction time96 h,and reaction temperature 55 ℃. Under these conditions,the conversion rate of camphene was 89. 5% and the selectivity of diisobornyl oxalate was 95. 6%. The structure of diisobornyl oxalate was characterized by IR,LCMS-IT-TOF,1H NMR and13 C NMR.