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Gas antisolvent fractionation based optical resolution of ibuprofen with enantiopure phenylglycinol
Journal of CO2 Utilization ( IF 7.7 ) Pub Date : 2018-09-08 , DOI: 10.1016/j.jcou.2018.09.004
L. Lőrincz , Á. Tóth , L. Kondor , O. Kéri , J. Madarász , E. Varga , E. Székely

Optical resolution is still the dominant route to obtaining enantiopure active ingredients. The traditional methods require large organic solvent quantities and long processing times. Antisolvent fractionation with supercritical carbon dioxide offers intensified processing by drastically reducing the time requirement of the diastereomeric salt precipitation. A novel optical resolution of ibuprofen was developed and optimized with phenylglycinol as a resolving agent and gas antisolvent fractionation as the separation method. Above the critical values of certain operational parameters (carbon dioxide to methanol ratio, apparent diastereomeric salt concentration, equilibration time, the relative volume of the extracting fluid) the selectivity was roughly constant, the optical resolution is robust. The scalemic mixtures were purified by repeated resolution and enantiomeric purities above 99% were reached in three consecutive steps.



中文翻译:

基于气体反溶剂分馏的布洛芬与对映体纯苯甘醇的光学拆分

光学拆分仍然是获得对映纯活性成分的主要途径。传统方法需要大量的有机溶剂和较长的处理时间。超临界二氧化碳的反溶剂分馏可通过大大减少非对映异构体盐沉淀的时间要求来提供增强的工艺。开发了一种新型的布洛芬光学拆分物,并以苯基甘醇作为拆分剂,采用气体反溶剂分馏作为分离方法进行了优化。高于某些操作参数的临界值(二氧化碳与甲醇的比率,表观非对映异构体盐浓度,平衡时间,萃取液的相对体积)时,选择性大致恒定,光学分辨率稳定。

更新日期:2018-09-08
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