摘要
松油醇副产物在催化剂磷酸和助催化剂碘作用下催化异构同时与马来酸酐发生Diels-Alder反应,生成1-异丙基-4-甲基二环[2,2,2]-5-辛烯-2,3-二酸酐(TMA)。运用正交实验确定了合成TMA的最佳合成条件:反应温度155℃,催化剂质量分数为1.5%,助催化剂质量分数为0.05%,n(副产物主成分)∶n(马来酸酐)=2.2∶1,反应时间为2 h,在该条件下,TMA的收率为86.2%。利用红外光谱、核磁共振氢谱、质谱等方法对TMA结构进行了表征。
1-Isopropyl-4-methylbicyclooct-5-ene-2,3-dicarboxylic anhydride（TMA） was prepared via the isomerization of terpineol by-products followed by the Diels-Alder reaction with maleic anhydride in the presence of phosphate catalysis.The optimum conditions were found by orthogonal tests to be as follows： reaction temperature 155 ℃,catalyst mass fraction of 1.5%,cocatalyst mass fraction of 0.05%,n（by-product of principal component）∶n（maleic anhydride）=2.2∶1,and reaction time of 2 hours.The yield of TMA amounted to 86.2%.The structure of the TMA was analyzed and characterized by IR,1HNMR and MS.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2010年第5期509-511,共3页
Fine Chemicals
基金
广西林产化学品开发与应用重点实验室开放基金项目(GXFC08-10)~~
