✦ LIBER ✦

Separation of pyridine derivatives from synthetic mixtures by pH-zone-refining counter-current chromatography

✍ Scribed by Shengqiang Tong; Jizhong Yan; Jian Li; Jianzhong Lou

Publisher: John Wiley and Sons
Year: 2007
Tongue: English
Weight: 463 KB
Volume: 30
Category: Article
ISSN: 1615-9306
DOI: 10.1002/jssc.200700062

No coin nor oath required. For personal study only.

✦ Synopsis

Abstract

Three novel pyridine derivatives were successfully separated from their partially purified synthetic mixtures by pH‐zone‐refining counter‐current chromatography using a multilayer coil planet centrifuge designed in our laboratory. After equilibration of a two‐phase solvent system consisting of methyl tert‐butyl ether–tetrahydrofuran–water at an optimized volume ratio of 4:6:7, triethylamine (10 mM) was added to the organic phase as a retainer and hydrochloric acid (10 mM) to the aqueous phase as an eluter. Separation runs of 1.20, 1.16, and 1.15 g of three samples yielded three pyridine derivatives in weights of 306, 255, and 314 mg at a high purity of over 98.5, 99.0, and 98.2% (determined by HPLC), respectively. The structures were identified by electron impact mass spectrometry and ^1^H NMR.

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