摘要
在DLB催化下,α-蒎烯经异构同时和马来酸酐发生D iels-A lder反应制备1-异丙基-4-甲基二环[2.2.2]-5-辛烯-2,3-二酸酐(TMA)。运用正交试验法研究了影响合成TMA的主要因素:反应温度、催化剂种类、催化剂用量、反应时间,并确立其最佳合成条件:催化剂用量3%(以α-蒎烯的质量计),反应温度145℃,反应时间1.0 h,(反应物α-蒎烯与马来酸酐摩尔比为1.4∶1)。TMA的收率达88%以上,纯度达92%以上,并明显缩短了反应时间。此外,利用红外光谱、薄层色谱、气相色谱和GC-MS等方法对TMA进行了分析和表征。
1-Isopropyl- 4-methyl bicyclo [ 2.2.2 ] oct-5-ene-2,3-dicarboxylic anhydride （ α-terpinene-maleic anhydride adduct, TMA） was prepared via isomerization of α-pinene followed by Diels-Alder reaction with maleic anhydride in the presence of DLB catalyst. Influence factors such as reaction temperature, dosage and variety of catalyst and reaction time were studied, and the optimum conditions were found by orthogonal tests to be as follows： reaction temperature 145 ℃, dosage of catalyst DLB 3 % （based on the weight of α-pinene）, reaction time 1.0 h （ molar ratio 1.4 ： 1 of α-pinene to maleic anhydride）. The yield of TMA amounted to 88 % and the purity was up to 92 %. The TMA was analyzed and characterized by IR, TLC, GC and GC-MS.
出处
《生物质化学工程》
CAS
2006年第3期25-28,共4页
Biomass Chemical Engineering
