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Separation and purification of intermediates for the preparation of naproxen from synthetic mixtures by countercurrent chromatography
Author(s) -
Qiu Xujun,
Lv Liqiong,
Sun Wenyu,
Wang Chaoyue,
Yan Jizhong,
Tong Shengqiang
Publication year - 2018
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.201800234
Subject(s) - countercurrent chromatography , chemistry , chromatography , column chromatography , countercurrent exchange , naproxen , hexane , solvent , methanol , organic chemistry , medicine , physics , alternative medicine , pathology , thermodynamics
Three key intermediates in the preparation of the nonsteroidal anti‐inflammatory drug naproxen were successfully separated and purified with high purity from synthetic mixtures by countercurrent chromatography with a selected biphasic solvent system. The biphasic solvent system composed of n ‐hexane/ethyl acetate/methanol/water (9:1:9:1, v/v/v/v) was selected according to partition performance of the three components using thin‐layer chromatography. Fifty milligrams of the synthetic mixture after the three‐step reaction was injected into a preparative countercurrent chromatography separation column and yielded 3.5, 14.0, and 8.0 mg of three key intermediates with 95.0, 99.0, and 98.0% purity, and the recovery of each component was 65.2, 71.2, and 69.6%, respectively. The results indicated that countercurrent chromatography is an efficient alternative and economical method for the separation and purification of intermediate components from synthetic mixtures.