Some of the major challenges faced by researchers (and in particular – organic and analytical chemists) include the need to quickly determine reaction kinetics as well as gain sufficient information to fully understand, characterize and optimize chemical reactions. This is leading researchers to find innovative ways to obtain the information they require to successfully complete their work.
I recently had a chance to meet with Danny Levin, President at Norac Pharma, during the 21st International Conference on Organic Process Research & Development (Scientific Update), January 2010, San Diego, CA.
After my presentation at the Organic Process Research & Development (OPRD) conference, Danny Levin described a paper he published a few years ago when he was head of research at NPIL Pharma Torcan (Org. Process Res. Dev., 2006, 10(6), pp 1296–1298). I had already used Danny Levin’s paper several times in my conference talks (figure 1) to illustrate the power of heat flow (Tr-Tj) at small scale, and Danny graciously provided some additional insight:
“I thought you might be interested in a publication of my own where I used METTLER TOLEDO MultiMax to good purpose in identifying and mitigating process scale up safety concerns during process development of a Horner Wadsworth Emmons reaction […]
The situation with the case study that I published was that we had been given a chemistry procedure that was believed by the originator to be safe and under control by virtue of slow addition of reagents. The MultiMax plot of (Tr-Tj) showed that this wasn’t the case – reagents were accumulating and the reaction and all the significant heat output occurred during warming for work-up!!!
It was the MultiMax data that quickly demonstrated the scale up hazard and allowed us to define a safely scaleable process. This critical aspect was not obvious from the presentation summary you kindly sent. You may wish to emphasize this point in future presentations to demonstrate the role of MultiMax in identifying and highlighting unsafe chemistry”.
As part of the on-going Recent Advances in Organic Chemistry by Academia Using Real-Time In Situ FTIR online seminar series, Dominique Hebrault will review recent advances in organic chemistry where real-time mid-infrared (mid-IR) analytics played a role in the advancement of organic chemistry research. This will take place on Wednesday, March 10.
Research topics include:
Advances in metal-catalyzed chemical transformations
Heterobimetallic for metal carbenoid chemistry as described by Huw M.L. Davies and colleagues at Emory University (United States)
Organolithium transformation from Vito Capriati, Saverio Florio, and colleagues from the University of Bari (Italy)
Palladium-catalyzed cross-coupling reactions as reported by Aiwen Lei and colleagues at Peking University (China)
Ruthenium-catalyzed dynamic kinetic resolution as described by Jan-E. Backvall and colleagues at Stockholm University (Sweden)
Highly selective polymerization reactions from Donald J. Darensbourg and colleagues at Texas A&M University (United States)
Chemical reactions in supercritical CO2 and system characterization from Paul A. Charpentier and colleagues at University of Western Ontario
Visit the Recent Advances in Organic Chemistry by Academia Using Real-Time In Situ FTIR online seminar page for more information.
Ian Clegg, an Associate Research Fellow at Pfizer Global Research and Development Sandwich Laboratories, United Kingdom recently posted a discussion on LinkedIn’s Process Analytical Technology (PAT) group site titled “PAT data (Mid-IR) posted onto YouTube.”
This YouTube video is entitled “Process Analytical Technology: Using Mid-IR spectroscopy to monitor a telescoped chemical reaction.”
In this video, 3 sequential chemical reactions are run in one vessel without stopping or isolating between reactions, and ReactIR™ (real-time in situ reaction analysis) is used to monitor all 3 reaction phases. All of the key reagents, intermediates and products produce unique peaks which show reaction progression without having to take samples. The video shows the spectra of the reaction as a function of time and how the spectra change. The video shows clearly which peaks were monitored and to which components those peaks correlate.