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Synthesis of Cellulose-23-bis(35-dimethylphenylcarbamate) in an Ionic Liquid and Its Chiral Separation Efficiency as Stationary Phase

机译:离子液体中纤维素23-双(35-二甲基苯基氨基甲酸酯)的合成及其固定相的手性分离效率

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摘要

A chiral selector of cellulose-2,3-bis(3,5-dimethylphenylcarbamate) (CBDMPC) was synthesized by reacting 3,5-dimethylphenyl isocyanate with microcrystalline cellulose dissolved in an ionic liquid of 1-allyl-3-methyl-imidazolium chloride (AMIMCl). The obtained chiral selector was effectively characterized by infrared spectroscopy, elemental analysis and 1H NMR. The selector was reacted with 3-aminopropylsilanized silica gel and the CBDMPC bonded chiral stationary phase (CSP) was obtained. Chromatographic evaluation of the prepared CSPs was conducted by high performance liquid chromatographic (HPLC) and baseline separation of three typical fungicides including hexaconazole, metalaxyl and myclobutanil was achieved using n-hexane/isopropanol as the mobile phase with a flow rate 1.0 mL/min. Experimental results also showed that AMIMCl could be recycled easily and reused in the preparation of CSPs as an effective reaction media.
机译:通过使3,5-二甲基苯基异氰酸酯与微晶纤维素溶于溶解在1-烯丙基-3-甲基咪唑鎓离子液体中的微晶纤维素反应,合成了2,3-双(3,5-二甲基苯基氨基甲酸酯)纤维素的手性选择剂(AMIMC1)。所得到的手性选择剂通过红外光谱,元素分析和 1 1 H NMR进行了有效表征。使选择剂与3-氨基丙基硅烷化的硅胶反应,得到CBDMPC键合的手性固定相(CSP)。通过高效液相色谱(HPLC)对制备的CSP进行色谱评估,并使用正己烷/异丙醇作为流动相,以1.0 mL / min的流速实现三种典型杀菌剂(包括六康唑,甲霜灵和霉菌丁)的基线分离。实验结果还表明,AMIMC1可以很容易地回收利用,并可以在制备CSP中用作有效的反应介质。

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