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Separation and purification of intermediates for the preparation of naproxen from synthetic mixtures by countercurrent chromatography

Qiu, Xujun, Lv, Liqiong, Sun, Wenyu, Wang, Chaoyue, Yan, Jizhong, Tong, Shengqiang
Journal of separation science 2018 v.41 no.14 pp. 3003-3008
acetates, countercurrent chromatography, methanol, nonsteroidal anti-inflammatory agents, solvents, thin layer chromatography
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.