马来松香酸制备新方法的研究
A New Method for Preparation of Maleic Rosin Acid
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摘要: 以松香和马来酸酐为原料制备马来松香酸。采用单因素试验法考察了不同反应条件对马来松香制备反应的影响,得出最佳反应条件为:马来酸酐与松香的物质的量比为1.1∶1,反应温度 190 ℃,反应时间 4 h,通过IR和单晶X射线衍射对马来海松酸酐结构进行表征,其构型为经典的二萜类化合物类型。用钾盐法对所制备的马来松香进行水解和纯化,得到纯度为95.3 %的马来松香酸,得率81.5 %,并利用IR、 1H NMR、 13C NMR 和MS对其结构进行确认。Abstract: Maleic rosin acid was prepared using rosin and maleic anhydride as raw materials. Effects of different reaction conditions on the reaction were investigated by single factor experimentation, and the optimum conditions were found to be as follows: mole ratio of maleic anhydride to rosin 1.1∶1, reaction temperature 190 ℃, reaction time 4 h. The structure of maleopimaric acid anhydride was characterized by IR and single crystal X-ray diffraction. It was found that the configuration of maleopimaric acid anhydride was the classical type of diterpene compounds. The prepared maleic rosin was hydrolyzed and purified by potassium salt method to obtain maleic rosin acid with purity of 95.3% and yield of 81.5%. The structure of maleic rosin acid was verified by means of IR, 1H NMR, 13C NMR and MS.
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