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

Author:
Qiu, Xujun, Lv, Liqiong, Sun, Wenyu, Wang, Chaoyue, Yan, Jizhong, Tong, Shengqiang
Source:
Journal of separation science 2018 v.41 no.14 pp. 3003-3008
ISSN:
1615-9306
Subject:
acetates, countercurrent chromatography, methanol, nonsteroidal anti-inflammatory agents, solvents, thin layer chromatography
Abstract:
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.
Agid:
6064604