HPLC法监控邻三氟甲基苯甲醚生产中的重氮化反应

Monitoring Diazo Reaction in Production Process of 2-(Trifluoromethyl) anisole by HPLC

研究了用高效液相色谱法监控以邻三氟甲基苯酚为原料合成邻三氟甲基苯甲醚的重氮化反应进程。采用hypersil ODS C18（4.6 mm×250 mm×5μm）色谱柱,以乙腈∶水（体积比60∶40）为流动相,检测波长为288 nm,流速为1.0 m L/min。结果表明,该监控方法在0.126-1.478 mg·m L-1内线性良好（相关系数r=0.9941）;加标平均回收率为95.39%,重复进样的RSD为0.62%-1.17%,该方法用于正交试验进程监控,重氮化反应最佳工艺条件为反应时间90 min,邻三氟甲基苯胺︰亚硝酸钠摩尔比为1∶1.1,原料反应率达到最高。

HPLC was applied to monitor the concentration of 2-（Trifluoromethyl） phenol in the synthesis process of2-（Trifluoromethyl） anisole,which is an important diazo reaction. Chromatography conditions were as follows： using hypersil ODS C18column（4. 6 mm × 250 mm × 5 μm）,mobile phase was acetonitrile ∶ water = 60 ∶ 40,detection wavelength was 288 nm,flow rate was 1. 0 m L·min-1. The results showed that the plot of the content and the peak area displays good linearity in the range of 0. 126 - 1. 478 mg/m L of esterification reaction mixture with r = 0. 9941,the average recovery was 95. 39% while the relative standard deviation for repetitions was 0. 62% - 1. 17%. This method has the advantages of high accuracy,good precision and good actual monitoring effect.