薄层色谱法应用于N-乙基-对-薄荷烷-3-甲酰胺的分离和鉴别

Thin Layer Chromatographic Separation and Characterization of N-Ethyl-p-Menthane-3-Carboxamide

研究了用薄层色谱法分离和鉴别在合成N-乙基-对-薄荷烷-3-甲酰胺中所得粗品的各组分。试验表明硅胶H(60型)为最佳吸附剂。敷有此吸附剂的薄层层析板经在110℃活化2 h,所用展开剂为以5与1之比混合的石油醚和丙酮混合溶剂,展开距离最少为14.00 cm,经展开后粗品中4组分得到很好的分离。展开层用碘铋化钾(KBI4)溶液和碱性高锰酸钾溶液喷洒即可清楚地观察到4个色斑,其Rf值依次为0.82,0.67,0.50和0.33,即Rf为0.33的色斑取下作元素分析,所得结果证明此组分即是N-乙基-对-薄荷烷-3-甲酰胺。

Conditions of TLC separation and characterization of crude product in the synthesis of N-Ethyl-p- menthane-3-carboxamide were studied. Silicagel H （type 60） was used as adsorbent supported on the thin layer chromatographic plate, which was activated at 110 ＂C for 2 h. Mixed solvent containing petroleum ether and acetone in the ratio of 5 to 1 （by volume） was used as eluant, with least eluting distance of 14. 00 cm, and 4 components in the crude product were well separated. By spraying the developed thin layer with potassium iodobismuthate （KBiI4） solution and alkaline potassium permangnate （KMnO4） solution as color reagents, 4 colored spots were observed clearly with their Rf values of 0. 82, 0. 67, 0. 50 and 0. 33. The component of the spot with Rf 0. 33 was taken for elementary analysis, and as shown by the analytical results, the component was proved to be the N-ethyl-p- menthane-3-carboxamide.