The Wrangler Group LLC

A manufacturer of energetic compounds needed to scale up a process, which involved explosive intermediates and final product. The batch process on a small scale contained significant risk of explosion due to detonation of the batch mixture due to compound splashing on the interior of the mixing vessel and drying out of the intermediate formed in the reaction. A continuous flow system was designed (picture below) to manufacture one of the compounds in this series at a scale of 30 g/hr. The system contained three pumps, an interdigitated mixer and a residence time loop fitted with temperature control capability. The reaction formed a gas and thus a phase separator was included to remove the gas continuously. On line monitoring was provided in the form of pH, flow, temperature, pressure, UV and leak detection.

The entire system was controlled by software remotely such that the operator did not need to be present in the production bay thus further mitigating the risk. Included in the system was a clean-in-place module also under software control. A cleaning regime was automatically programmed between each production run and always before system shut down. The first unit was deployed successfully followed by several orders for prodcution units.

The entire system was mounted on a portable platform capable of passing through a typical laboratory door to facilitate ease of transport between production facilities. In addition, reception vessels were designed such that the product could be continuously removed throughout the production run to facilitate analysis and further processing. As part of the project an analysis system consisting of an HPLC with LC/MS detection was designed to provide complete quantitation of reagents, intermediates and final product.

A customer involved in medicinal chemistry needed a fully automated system which would handle a broad range of compounds. The system needed to scan the reaction mixture initially on a small scale, then developed an optimized HPLC method to purify a compound of interest and using the optimized method, purify a large amount of reaction mixture in one run. A system was designed to do this (picture below) with a purification scale up capability from 50 mg to 50 grams.

The system was controlled by software, which allowed the system to run unattended. The separations units contained many columns to separate reaction mixtures and recover purified product. Included in the system are; 4 preparative chromatographic pumps; two analytical chromatographic pumps; two dual arm autosamplers with temperature controlled sample handling capability; valve switching module; two UV detectors; one MS detector; one fraction collector; solvent and waste containers. The system is used continuously to screen and purify compounds of medicinal interest.