Automated Sampling for Chemical Reactions

Pipettes and syringes are common laboratory tools to take manual samples. The challenges with pipettes and syringes are reproducibility, consistency, presence and availability.

These challenges together with the need for automation and standardization in the laboratory inspired us to develop an automated sampling solution for a wide range of chemical reactions. EasySampler is an automated, unattended technology delivering high quality analytical samples day and night. The probe-based technology has a micro-pocket, which takes samples at any given time, quenches in-situ and dilutes for ready to analyze offline samples.

Automated sampling technology is key to doubling productivity in the laboratory, since sampling and experimentation can now be done around the clock. ​

The EasySampler supports reaction understanding by providing samples on demand. Sampling is performed under reaction conditions, making it truly representative. The samples, once collected and time stamped, can be analyzed via offline analytical methods and the result integrated back into the data stream. An additional value lies in the increased data quality through automatic and seamless data collection. Increased accuracy and precision provides higher quality results versus manual sampling.

The fully automated and unattended EasySampler boosts your productivity in the lab. The simple and intuitive touchscreen allows scientists to schedule as many sample collections needed, providing reliable data day and night. This will allow you to never miss a sample again. ​

Operated individually, EasySampler can be preprogrammed with 
sampling and dilution sequence allowing samples at defined times.

EasySampler can be seamlessly integrated with chemical reactors, including EasyMax, OptiMax, RX-10 or RC1mx. Samples can be taken depending on other reaction parameters or attributes, including temperature, stirring, dosing, pH or other PAT related information. 

Traditionally, many experiments have been performed during the regular working hours. Therefore, workflows were designed around presence and availability. These lead to blind spots, information and understanding gaps.

EasySampler allows fit-for-purpose experimentation and changes the way scientists work, allowing offline analysis samples 24/7. Researchers only need to adopt to a minor change in their workflow: schedule the sampling sequence first and then start your experiment.

EasySampler automated sampling technology is convenient to use, allowing for effortless planning and experiments. 

Laboratories typically operate with intensity during the day, but slow down or shut down during the night. Experiments are inefficiently scheduled as scientists must be present to take samples or change process variables.

A scientist's workflow can be optimized from end-to-end using platform technologies that eliminate non-value added tasks and manage the data that is collected. Experiments can now be scheduled around the clock and samples can be taken automatically anytime Data can be collected for every single experiment and can be automatically stored and shared, according to the needs of the organization. 

Three simple steps, when combined into one single operation, are powerful. EasySampler is disrupting the way chemist work:

1. Accurate sampling starts with immersion of the micro-pocket
2. Immediate quench stops the reaction and ensures the time point is representative 
3. Subsequent dilution and dispensing in the vial ready for offline analysis

These steps take your samples to the next level of reproducible and representative analytical results. Above all, automated samples are now taken at preprogrammed or scheduled times. 

Sample chemical reactions in an easy and safe way. The micro-pocket is exposed to chemistry, not you. 

When working in the laboratory, you are potentially exposed to hazardous chemicals. and are at risk for injury. When taking samples manually, the operator needs to open the reactor, and can be exposed to toxic materials at elevated temperatures. EasySampler eliminates manual handling and exposure to hazardous chemicals. Therefore, this reduces risks and improves operator safety. 

For heterogeneous, multiphase and slurry chemical reactions, manual sampling is challenging. With EasySampler, those reactions can be sampled, even under various reaction conditions. 

Highly reactive chemistry, viscous and slurry reaction mixtures, toxic and hazardous substances are challenging when it comes to sampling. EasySampler can take samples from a wide variety of reactions, automated and unattended. 

Samples from EasySampler are representative and reproducible, using a method that reinvents sampling with 3 individual steps combined in a single operation.

Elevate your R&D to the next level of understanding and catalyze your research with automated and unattended chemistry sampling solutions. 

Reactions with atmospheres from inert gas for air- and water-sensitive chemistries to pressurized reactions, such as hydrogenation reactions, are difficult to sample. Studying these types of reactions is tedious and time-consuming, unless automated and unattended technology is employed. The micro-pocket EasySampler technology is immersed in the liquid phase, and effortlessly takes samples under various reaction conditions. 

• Impurity Profiling
• Parallel Synthesis
• Organometallic Synthesis and Chemistry
• Chemical Reaction Kinetics
• Design of Experiments
• Synthesis Reactions
• Flow Chemistry
• High Pressure Reactions
• Hydrogenation Reactions
• Quality by Design

Continued automated sampling with the EasySampler supports reaction and impurity profiling studies. A list of publications from peer-reviewed journals focuses on exciting and novel applications of EasySampler by researchers in both academia and industry to support data-rich experimentation to advance their research.

• Malig T.C., Tan Y., Wisniewski S.R., Higman C.S., Carrasquillo-Flores R., Ortiz A., Purdum G.E., Kolotuchin S. and Hein J.E., " Development of a telescoped synthesis of 4-(1H)-cyanoimidazole core accelerated by orthogonal reaction monitoring", React. Chem. Eng. (2020), 5, 1421-1428
  
  
• Wang, K., Han, L., Mustakis, J., Li, B., Magano, J., Damon,D., Dion, A., Maloney, M.T., Post, R.J., Li, R., "Kinetic and Data Driven Reaction Analysis for Pharmaceutical Process Development", Ind. Eng. Chem. Res. (2019), Advance article
  
  
• Beutner, G.L., Coombs, J.R., Green, R.A., Inankur, B., Lin, D., Qiu, J., Roberts, F., Simmons, E.M., Wisniewski, S.R., "Palladium-Catalyzed Amidation and Amination of (Hetero)aryl Chlorides under Homogeneous Conditions Enabled by a Soluble DBU/NaTFA Dual-Base System", Org. Process Res. Dev. (2019), 23, 1529-1537.
  
  
• Mennen, S.M., Alhambra, C., Allen, C.L., Barberis, M., Berritt, S., Brandt, T.A., Campbell, A.D., Castañón, J., Cherney, A.H., Christensen, M., Damon, D.B., de Diego, J.E., García-Cerrada, S., García-Losada,P., Haro, R., Janey, J., Leitch, D.C., Li, L., Liu, F.,  Lobben, P.C., MacMillan, D.W.C., Magano, J., McInturff, E., Monfette, S., Post, R.J., Schultz, D., Sitter, B.J., Stevens, J.M., Strambeanu, I.I., Twilton, J., Wang, K., Zajac, M.A., "The Evolution of High-Throughput Experimentation in Pharmaceutical Development and Perspectives on the Future", Org. Process Res. Dev. (2019) 23, 1213−1242.
  
  
• Carter, H.L.,  Connor, A.W., Hart, R., McCabe, J., McIntyre, A.C., McMillan, A.E., Monks, N.R., Mullen, A.K., Ronson, T.O., Steven, A., Tomasia, S., Yates, S.D., "Rapid route design of AZD7594", React. Chem. Eng. (2019), Advance Article.
  
  
• Zawatzky, K., Grosser, S., Welch, C.J., "Facile Kinetic Profiling of Chemical Reactions Using MISER Chromatographic Analysis", Tetrahedron, (2017) 73, 5048-5053.
  
  
• Gurung, S.R., Mitchell, C., Huang, J., Jonas, M., Strawser, J.D., Daia, E., Hardy, A., O’Brien, E., Hicks, F., Papageorgiou, C.D., "Development and Scale-up of an Efficient Miyaura Borylation Process Using Tetrahydroxydiboron", Org. Process Res. Dev. (2017) 21, 65-74.
  
  
• Rougeot, C., Situ, H., Cao, B.H., Vlachos, V., Hein, J.E., "Automated Reaction Progress Monitoring of Heterogeneous Reactions: Crystallization-induced Stereoselectivity in amine-catalyzed aldol reactions", React. Chem. Eng. (2017), 2, 226-231.
  
  
• Malig, T.C., Koenig, J.D.B., Situ, H., Chehal, N.K., Hultinb, P.G., Hein, J.E., ”Real-time HPLC-MS reaction progress monitoring using an automated analytical platform", React. Chem. Eng. (2017) 2, 309-314.
  
  
• Duan, S., Place, D., Perfect, H.H., Ide, N.D., Maloney, M., Sutherland, K., Price Wiglesworth, K.E.; Wang, K., Olivier, M., Kong, F., Leeman, K., Blunt, J., Draper, J., McAuliffe, M., O’Sullivan, M., Lynch, D. , Palbociclib Commercial Manufacturing Process Development. Part I: Control of Regioselectivity in a Grignard-Mediated SNAr Coupling", Org. Process Res. Dev. (2016), 20, 1191−1202.
  
  
• Nykaza, T. V.; Ramirez, A.; Harrison, T. S.; Luzung, M. R.; Radosevich, A. T., Biphilic Organophosphorus-Catalyzed Intramolecular Csp2–H Amination: Evidence for a Nitrenoid in Catalytic Cadogan Cyclizations. Journal of the American Chemical Society 2018, 140 (8), 3103-3113.