摘要
利用柱层析法分离2,5-二甲基十四烷基苯同系物,首先用薄层板进行点样,根据板上点的个数确定待分离的物质所含化合物的种类,以此确定所要的组分,并通过各点的距离初步确定洗脱液的极性配比;然后对样品进行柱层析分离,在洗脱过程中,根据不同极性物质谱带距离的不同,分别收集,并通过薄层板监控,确定所需谱带,再经旋转蒸发仪去除洗脱液,得到所要的纯净物.确定了最佳的展开剂体系体积比为:V(正己烷):V(四氯化碳):V(氨水)=3:1:0.2,利用核磁氢谱(1HNMR)和气质联用(GC-MS)法验证了纯化后产物的化学结构与分子设计相符.
In this paper the column chromatography was utilized to separate series of 2,5-dimethyl tetradecyl benzene isomers compounds.Firstly,the thin layer chromatography was used to analyze the kind of the compound what we need according to the number of the point.And the polarity of the eluant was confirmed by the distances between those points.Then 2,5-dimethyl tetradecyl benzene isomers compounds could be separated.In the process of elution,different compounds had different bands and the wanted band could be collected by supervising.Eluant was evaporated through rotatory evaporator.The collected compounds were obtained pure product,the optimum developer was V(hexane):V(tetrachloride):V(ammonia)=3:1:0.2.Then the structures of the purified products were characterized by 1H NMR and GC-MS proved as being expected.
出处
《大庆石油学院学报》
CAS
北大核心
2010年第2期92-96,共5页
Journal of Daqing Petroleum Institute
基金
国家"973"重点基础研究发展计划项目(2005CB221305)
黑龙江省研究生创新科研项目(YJSCX2008-044HLJ)
关键词
2
5-二甲基十四烷基苯
薄层色谱
柱层析
展开剂
分离
2,5-dimethyl tetradecyl benzene
thin-layer chromatography
column chromatography
developer
separation
