Separation of acetylferrocene from synthetic mixtures by countercurrent chromatography

IF 1 4区化学 Q4 BIOCHEMICAL RESEARCH METHODS

Journal of Liquid Chromatography & Related Technologies Pub Date : 2022-05-09 DOI:10.1080/10826076.2022.2143798

Xiao‐yong Lv, Haibo You, Huiyun Qiu, Mengyi Wen, Chuncui Zheng, Shengqiang Tong

引用次数: 0

Abstract

Abstract The main product of acetylation of ferrocene was successfully separated and purified with high purity from synthetic mixtures by countercurrent chromatography using a selected biphasic solvent system. According to distribution performance of main product and reactant, a two-phase solvent system was selected by thin layer chromatography, in which the partition coefficient for each component was determined by HPLC. Then a two-phase solvent system consisting of petroleum ether/ethyl acetate/methanol/water (6:4:6:4, v/v) was selected. After acetylation reaction, 20 mg of synthetic mixture was subjected to countercurrent chromatography, yielding 2.1 mg of ferrocene and 8.7 mg of acetyl ferrocene with 96.6% and 97.4% purity. Results indicated that countercurrent chromatography is a very efficient method for separation and purification of target product from synthetic mixtures. GRAPHICAL ABSTRACT

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逆流色谱法从合成混合物中分离乙酰二茂铁

摘要采用选择的双相溶剂体系，采用逆流色谱法，成功地从合成混合物中分离纯化了二茂铁乙酰化的主要产物。根据主要产物和反应物的分布性能，采用薄层色谱法选择了两相溶剂体系，并用高效液相色谱法测定了各组分的分配系数。然后选择由石油醚/乙酸乙酯/甲醇/水（6:4:6:4，v/v）组成的两相溶剂体系。乙酰化反应后，20 将mg合成混合物进行逆流色谱，得到2.1 mg二茂铁和8.7 mg乙酰基二茂铁，纯度分别为96.6%和97.4%。结果表明，逆流色谱法是从合成混合物中分离纯化目标产物的一种非常有效的方法。图形摘要

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来源期刊

Journal of Liquid Chromatography & Related Technologies 化学-分析化学

CiteScore

2.80

自引率

0.00%

发文量

审稿时长

4.9 months

期刊介绍： The Journal of Liquid Chromatography & Related Technologies is an internationally acclaimed forum for fast publication of critical, peer reviewed manuscripts dealing with analytical, preparative and process scale liquid chromatography and all of its related technologies, including TLC, capillary electrophoresis, capillary electrochromatography, supercritical fluid chromatography and extraction, field-flow technologies, affinity, and much more. New separation methodologies are added when they are developed. Papers dealing with research and development results, as well as critical reviews of important technologies, are published in the Journal.