松油醇副产物与马来酸酐催化异构/Diels-Alder反应的研究

Study of the Diels-Alder Reaction of Terpineol by-product Catalyzed isomerism and Maleic Anhydride

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0.08%，n(副产物主成分):n(马来酸酐)=2.2：1，反应时间为2h，TMA的收率为86.2%。并利用红外光谱、核磁共振、质谱等方法对TMA结构进行表征。

Abstract:

1-lsopropyl-4-methylbicyclo[2,2,2]oct-5-ene-2,3-dicarboxylic anhydride(TMA) was prepared via isomerization of terpineol-products followed by 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%, catalysts mass fraction of 0.08%, 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, NMR and MS.