低温催化剂关键中间体Ts_2-tacn的检测分析

Study on Ts_2-tacn,the Key Intermediate of Low Temperature Catalyst

实验根据Richman-Atkins法,综合文献报道的一些方法,以二乙烯三胺为起始原料,经磺酰化保护成环后脱Ts制得Ts_2-tacn。将该化合物用热乙醇洗涤三次烘干后进行红外分析、有机质谱分析、热重分析、核磁分析,以表征其结构;同时建立了HPLC法测试该化合物纯度的分析方法,以确定转化率以便计算下一步的投料,实验对仪器条件进行优化,并确定了最佳条件,在29374 mg/L回归方程为Y=1.2613x-0.1742,相关系数为0.9998,相对标准偏差小于1%,回收率在98%106%之间,结果表明本方法简单,快速,准确。

According to Richman-Atkins and some analysis determination methods,Ts_2-tacn was synthesized Ts_2-tacn was qualitative analyzed by FTIR,MS,DSC,1H NMR. An HPLC procedure was developed for determination of Ts_2-tacn,the operating conditions of HPLC were optimized. The recovery was in the range from 98% to 106% with relative standard deviation being less than 1%. The method is simple,efficient and accurate.