摘要
采用均匀设计方法深入研究了去氢枞酸甲酯在HNO3-Ac2O-AcOH体系中选择性硝化的反应条件。通过理论计算和实验验证获得去氢枞酸甲酯选择性硝化的较优反应条件如下:n(硝酸)∶n(去氢枞酸甲酯)为3∶1、混合溶剂中乙酐与乙酸的体积比为7∶1、反应温度为20℃、反应时间为60 min。此时12-硝基去氢枞酸甲酯和14-硝基去氢枞酸甲酯的总产率由50%提高到84.6%,其中12-硝基去氢枞酸甲酯的产率达到64.0%、14-硝基去氢枞酸甲酯的产率达到20.6%,二者的产率比约为3.1∶1。12-硝基去氢枞酸甲酯的反应产率和选择性都明显高于文献报道值。
The regioselective nitration of methyl dehydroabietate in the reaction system of HNO3-Ac2O- AcOH had been deeply explored by use of the uniform design experiments. The optimum reactive conditions of the regioselective nitration of methyl dehydroabietate had been obtained by the theoretic calculation and the proving tests. When the molar ratio of HNO3 to methyl dehydroabietate was 3 ： 1,the volume ratio of Ac2O to AcOH was 7 ： 1 ,the reaction temperature was 20℃ ,and reaction time was 60 min,the total yield of methyl 12- nitrodehydroabietate and methyl 14-nitrodehydroabietate increased from 50% to 84.6% ,among which the yield of methyl 12-nitrodehydroabietate was high up to 64.0% and the yield of methyl 14-nitrodehydroabietate reached 20.6% with a yield ratio of 3.1 ： 1. Compared with the data of the references,the reaction yield and the regioselectivity of the nitration of methyl 12-nitrodehydroabietate was obviously promoted.
出处
《化学与生物工程》
CAS
2008年第6期33-37,共5页
Chemistry & Bioengineering
