CAJ | 학술논문

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。
통과감희화초산재붕항최화작용하적중배가성(지화)반응합성료초산이이용뇌지,탐토료원료배비、최화제용량、반응온도이급반응시간대지화반응적영향。연구결과표명,감희(13.6 g)、초산화최화제적질량비위1.7∶2∶1,반응온도위55℃、반응시간위96 h적조건하,감희적전화솔위89.5%,초산이이용뇌지적선택성위95.6%。산물통과IR、LCMS-IT-TOF、1H NMR、13C NMR등수단진행료결구감정여표정。
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 time 96 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 and 13C NMR.