无溶剂法合成1,6-六亚甲基二氨基甲酸甲酯

SOLVENT-FREE SYNTHESIS OF DIMETHYLHEXANE-1,6-DICARBAMATE

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%。

A new and green solvent-free syntheses of dimethylhexane-1, 6-dicarbamate from methylphenylearbonate 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-C18, 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%.