| 无溶剂法合成1,6-六亚甲基二氨基甲酸甲酯 |
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| 引用本文： | 邱志燕,杨勇,崔咪芬,汤吉海,陈献,乔旭.无溶剂法合成1,6-六亚甲基二氨基甲酸甲酯[J].精细石油化工,2010,27(5). |
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| 作者姓名： | 邱志燕 杨勇 崔咪芬 汤吉海 陈献 乔旭 |
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| 作者单位： | 1. 南京工业大学化学化工学院,江苏,南京,210009
2. 南京工业大学化学化工学院,江苏,南京,210009;南京工业大学材料化学工程国家重点实验室,江苏,南京,210009 |
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| 基金项目： | 国家"863"计划基金资助项目 |
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| 摘 要： | 研究了甲基苯甲碳酸酯和1,6-六亚甲基己二胺无溶剂法合成1,6-六亚甲基二氨基甲酸甲酯的绿色新工艺。建立了适用该反应体系的高效液相色谱定量分析方法,并优化了工艺条件。分析条件为:AgilentZORBAX SB-C18柱,流动相V(乙腈):V(水)=55:45,柱温为25℃,检测波长200 nm,流速0.8 mL/min。最佳工艺条件为:反应温度60℃,反应时间1 h,n(甲基苯甲碳酸酯):n(1,6-六亚甲基己二胺)=2.5:1,该工艺条件下,1,6-六亚甲基二氨基甲酸甲酯收率达99.6%。
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| 关 键 词： | 1 6-六亚甲基二氨基甲酸甲酯 己二胺 甲基苯基碳酸酯 无溶剂法 |
SOLVENT-FREE SYNTHESIS OF DIMETHYLHEXANE-1,6-DICARBAMATE |
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| Qiu Zhiyan,Yang Yong,Cui Mifen,Tang Jihai,Chen Xian,Qiao Xu.SOLVENT-FREE SYNTHESIS OF DIMETHYLHEXANE-1,6-DICARBAMATE[J].Speciality Petrochemicals,2010,27(5). |
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| Authors: | Qiu Zhiyan Yang Yong Cui Mifen Tang Jihai Chen Xian Qiao Xu |
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| Abstract: | A new and green solvent-free syntheses of dimethylhexane-1,6-dicarbamate from methylphenylcarbonate and 1,6-diaminohexane were studied. The quantitative analysis method by high performance liquid chromatography for the reaction was developed and the process conditions were optimized. Suitable analytical conditions were found as follows: column Agilent ZORBAX SB-C_(18),mobile phase V(acetonitrile):V(water) = 55:45,column temperature 25℃,detection wavelength 200 nm and flow rate 0.8 mL/min.Under the optimum reaction conditions: reaction temperature 60℃, time 1 h and n(methylphenylcarbonate):n(1,6-diaminohexane) = 2.5:1,the yield of dimethylhexane -1,6-dicarbamate could reach 99.6%. |
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| Keywords: | dimethylhexane-1 6-dicarbamate 1 6-diaminohexane methylphenylcarbonate solvent-free reaction |
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