文献类型：专利

英文题名：Separation of aminoglutethimide racemates using multi-column simulated moving bed chromatography comprises e.g. selecting the mobile phase and the chiral stationary phase for the resolution of the racemate, eluting the racemate solutions

作者：LI P;YU J;LIN X;YANG Y

机构：[1]UNIV EAST CHINA SCI & TECHNOLOGY

申请号：CN106390519-A

申请日：2016-09-12

公开日：2017-02-15

语种：英文

收录：DERWENT

摘要：NOVELTY - Separation of aminoglutethimide racemates using multi-column simulated moving bed chromatography comprises e.g. selecting the mobile phase and the chiral stationary phase for the resolution of the racemate, determining the simulated moving bed operating mode, operating the system to achieve a stable state, eluting in simulated moving bed extraction port and raffinate solution to obtain high purity R/S-aminoglutethimide solution, then concentrating the both solutions, recrystallizing, filtering, drying to obtain final product as powder. USE - The method is useful for separation of aminoglutethimide racemates using multi-column simulated moving bed chromatography (claimed). ADVANTAGE - The method is continuous and facilitates large scale production. DETAILED DESCRIPTION - Separation of aminoglutethimide racemates using multi-column simulated moving bed chromatography comprises (i) selecting the mobile phase and the chiral stationary phase for the resolution of the racemate, where the mobile phase is mixture of ethanol, n-hexane and ethanolamine and the chiral stationary phase is silica gel coated with cellulose - tris(3,5)-dimethylphenylcarbamate, (ii) determining the number of columns filled in each area to build a multi-column simulated moving bed structure, and determining the simulated moving bed operating mode, (iii) measuring the adsorption equilibrium and adsorption kinetics of the mixture of aminoglutethimide based on the experiment, designing the simulated moving bed separation area using triangular theory and the conditions of liquid and solid flow rate, where the design limit is that the purity of the single ammonium enantiomer reaches the desired set value, (iv) determining the flow rate of the packed column using design of the simulated moving bed separation operating area, then setting the material flow rate, feed concentration, switching time and operating temperature and other operating conditions, where operating temperature is 20-60 degrees C, (v) implementing simulated moving bed separation of arundinium racemates which is a dynamic adsorption separation system that requires multiple cycles, operating the system to achieve a stable state, when the system becomes stable to obtain high-purity R-aminoglutethimide enantiomer in the extraction port, S-aminoglutethimide enantiomer in the raffinate, and (vi) eluting in simulated moving bed extraction port to obtain high purity R- aminoglutethimide enantiomeric and eluting the raffinate solution to obtain high purity S-aminoglutethimide enantiomeric solution, then concentrating the both solutions, recrystallizing, filtering, drying to obtain final product as powder.