Production Scale Multi-Stage Process

Example 6 Production Scale Multi-Stage Process 

Again the target component is surrounded by both early- and late-eluting impurities. However, in contrast to the foregoing example, here a multistage process consisting of a batch separation followed by two SMB separations was applied. The first batch unit divided the complete feed into two fractions. The 

Sample Adsorbent Cyclic peptide from fermentation broth LiChrospher 100 RP-18e. 5 pm LiChrospher 100 RP-18. 12 pm 

Mobile phase Acetonitrile-water gradient Acetonitrile-water, isocratic 

Both fractions obtained from the first separation can be processed in subsequent SMB units where, again, the respective portion is split into two fractions. In this case fraction (a) is fed to a SMB unit and the target product is collected as extract. An SMB separation of fraction (b) leads to a raffinate stream containing the main product and the extract line where all impurities are collected. 

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Example 6 Production Scale Multi-stage Process 213... 

Carried out on a small multi-gram scale, the overall yield over the four recycle loops in the unoptimized process was 49% (based on the amount of racemate added throughout the investigation) compared to a traditional single-step resolution yield of -30% of the N-benzyl amine, demonstrating some improvement from an early stage. The product was isolated in 80-90% ee over each loop and required a final crystallization of the combined material from acetone to bring it up to the required specification. The main losses were to the imine, and, in a separate experiment, treatment of this under the SCRAM racemization conditions in the... 

A key concept in CONDEA s product development process is the controlled scale-up or new products from laboratory to commercial production. The gap between pilot production cmd full scale commercial production, typical for the manufacturing industry, is being bridged by a flexible multi-purpose semi-commercial unit of approx. 1200 mt per year capacity, where large scale conunercial samples can be manufactured during the developmental stage. This concept reduces scale-up factors to a reasonable ratio and helps to shorten the development of new raw materials for catalytic applications. 

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