通过反相固相萃取高效分离杯[4]间苯二酚杯芳烃的C-四甲基异构体

Efficient Separation of C-Tetramethylcalix[4]resorcinarene Conformers by Means of Reversed-Phase Solid-Phase Extraction.

作者信息

Pineda-Castañeda Héctor Manuel, Maldonado Mauricio, Rivera-Monroy Zuly Jenny

机构信息

Chemistry Department, Universidad Nacional de Colombia, Carrera 45 No 26-85, Building 451, Office 134, Bogotá11321, Colombia.

出版信息

ACS Omega. 2022 Dec 21;8(1):231-237. doi: 10.1021/acsomega.2c03218. eCollection 2023 Jan 10.

DOI:10.1021/acsomega.2c03218

PMID:36643487

原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC9835186/

Abstract

A reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed to study the conformer formation generated during the reaction for obtaining -tetramethylcalix[4]resorcinarene. The chromatographic method was used to design a strategy for purifying the reaction products, using solid-phase extraction columns (RP-SPE) and gradient elution. The chromatographic profiles of the cyclocondensation reaction between resorcinol and acetaldehyde show the presence of three products under the different reaction and precipitation conditions studied. Using RP-SPE, it was possible to enrich the products, which were later characterized by means of RP-HPLC and H nuclear magnetic resonance (NMR). This investigation explored and established a new method for RP-HPLC analysis and RP-SPE separation of conformational isomers obtained in the formation reaction of -tetramethylcalix[4]resorcinarene.

摘要

开发了一种反相高效液相色谱（RP-HPLC）方法，以研究在制备对四甲基杯[4]间苯二酚芳烃的反应过程中生成的构象异构体。该色谱方法用于设计一种使用固相萃取柱（RP-SPE）和梯度洗脱来纯化反应产物的策略。间苯二酚与乙醛之间的环缩合反应的色谱图表明，在所研究的不同反应和沉淀条件下存在三种产物。使用RP-SPE可以富集产物，随后通过RP-HPLC和氢核磁共振（NMR）对其进行表征。本研究探索并建立了一种新的方法，用于对在对四甲基杯[4]间苯二酚芳烃形成反应中获得的构象异构体进行RP-HPLC分析和RP-SPE分离。