新三氮烯类试剂的提纯及鉴定 Ⅰ.薄层层析法

The purification and identification of the new triazene reagents I. Thin layer chromatography(TLC)method

本文提出了用薄层层析法纯化三氮烯类试剂的新方法.用硅胶G制板,以环己烷∶石油醚∶乙酸乙酯=2∶2∶1体系为展开剂.纯化后试剂的有效成分含量可达91%以上,基本上能满足各种不同分析应用的要求.最后并对纯化的产品进行了结构证实(IR and^1HNMR法).

A new method for the purification of the new triazene reagents by thin layer chromatography(TLC) method (Silica gel as adsorbent, Cyclohexane: Petroleum ether: Ethyl acetate = 2∶2∶1 as developer)is reported in this paper. The effective component contents in raw product are 63～67%, but are>91% in the purified form by spectrophotometry. The purified form can meet the needs of of the various analysis. Furthermore, the structure of the reagents are identified by IR and ~1HNMR.