Dipartimento di Chimica, Materiali e Ingegneria Chimica, Politecnico di Milano, via Mancinelli 7, I-20131 Milano, Italy.
J Chromatogr A. 2010 Apr 23;1217(17):2840-6. doi: 10.1016/j.chroma.2010.02.048. Epub 2010 Feb 26.
The pharmaceutically relevant compound (RS,RS)-2-(2,4-difluorophenyl)butane-1,2,3-triol, an important intermediate in the production of different antifungal drugs, is synthesized in racemic form. For further use in the laboratory the compound has to be separated into its pure enantiomers. This work describes the different steps required to set up a chiral separation using intermittent simulated moving bed chromatography (I-SMB). Furthermore, the effect of feed concentration on the choice of the operating conditions is presented in the frame of the triangle theory. The experiments are carried out at increasing total feed concentration ranging from 3 to 15 g/L. The results demonstrate that a successful I-SMB separation could be carried out thus separating 4.5 g of the racemic mixture and fulfilling the specified purity specification of 98% for both enantiomers.
(RS,RS)-2-(2,4-二氟苯基)丁烷-1,2,3-三醇是生产不同抗真菌药物的重要中间体,以外消旋形式合成。为了在实验室中进一步使用,该化合物必须分离成其纯对映异构体。本工作描述了使用间歇模拟移动床色谱(I-SMB)建立手性分离所需的不同步骤。此外,在三角形理论的框架内提出了进料浓度对操作条件选择的影响。实验在总进料浓度从 3 增加到 15 g/L 的范围内进行。结果表明,可以成功进行 I-SMB 分离,从而分离 4.5 克外消旋混合物,并满足两种对映异构体均为 98%的指定纯度规格。