Differences from standard Atlas System • Additional fast response temperature probe Reactor and jacket temperature • Insulated oil connectors Minimizing heat fluctuations • Power supply with calibration heater Enable calibration steps in HFC and perform PCC • PC software upgrade Seamlessly perform calorimetry experiments
Atlas HD automated reactor system Powerful automated reactor platform, seamlessly Atlas 1 PC Software with Calorimetry upgrade used as standard jacketed reactor when calorimetry Create experiment recipes for standalone measurements aren’t required. Vacuum jacketed operations. The calorimetry step is designed as a vessels are necessary to maintain isothermal wizard, to set all important parameters before the conditions. setup. It will automatically include calibration steps. Atlas Calorimetry bundle Atlas Reporting software Includes all necessary modules to turn Atlas HD into Used for post experiment analysis. Compensates for a reaction calorimeter: enthalpy of addition, and allows for generation of RS232 enabled power supply and calibration reaction power and enthalpy in single click. • heater • Quick response RTDs for precise temperature control • Additional insulation for oil connectors
Atlas PC Software Suite with Calorimetry upgrade Atlas 1 PC software • Advanced software for advanced control of Atlas • Calorimetry wizard for easy set-up – define all parameters and safety limits in few minutes • Control wide array of hardware (dosing setups, pH and turbidity probes etc.) Atlas Reporting Software • Plot power and enthalpy data with a few clicks • Automatically correct for enthalpy of addition
Example Thermogram: Hydrolysis of Acetic Anhydride Run Ac 2 O used Measured Measured enthalpy (g) enthalpy (KJ) (KJ/mol) 1 33.05 19.2 59.25 2 33.05 19.93 61.5 3 33.12 20.98 64.61 Measured enthalpy (KJ/mol) Average 61.8 Std. Dev. 2.69 Literature Value 58.6
Excellent control: Sophisticated PID control Easy analysis: and powerful circulators result in accurate Easy to use software allows graphs of power and isothermal performance. enthalpy to be plotted with only a few clicks. Accurate: Quick: Vacuum jacketed vessels, automated Everything clicks together quickly and easily calibration and sensitive RTDs give extremely high without the need for tools. Vessels can be accuracy results. changed in under 1 minute. Walk away operation: Flexible: Automated gravimetric or volumetric reagents The same equipment and software can be used for additions are all made easy. HFC or PCC, allowing the chemist to pick the best method for the reaction, or simply used as standard jacketed reactor for everyday use.
Control up to 4 Atlas HD systems from 1 PC • Fully independent control over each reactor with process data logging • The Atlas HD systems can be identical or completely different, offering the same flexibility as stand-alone Atlas HD systems • Atlas Parallel software allows for multiple instances of Atlas software to be opened, assigning each instance to one reactor. • Data for each reactor is saved independently in its own .csv file
Fine control of your crystallizations Crystallisation process consists of two major events: • Nucleation • Crystal Growth Following the progress of a crystallisation process can allow chemists to tailor the properties of the crystals to suit their needs • Syrris offers two approaches: Monitor: Using Syrris Turbidity Node and Probe Control: Using Sonocrystallization technique
Turbidity Monitoring • Powerful tool for calculating metastable zone of a system • Turbidity has been used to measure and monitoring the subsequent crystallisation crystallisations for decades • • Works by measuring back-scattered light by Atlas can use turbidity signal to control other reaction suspended solids in a liquid parameters (e.g. stop dosing when turbidity exceeds X %) Crystallisation of Adipic Acid Dissolution of Adipic Acid 120 66 120 66 100 64 100 64 Power (watts) \ Turbidity (%) 80 62 80 62 Temperature (°C) Temperature(°C) Turbidity (%) 60 60 60 60 40 58 40 58 20 56 20 56 0 54 0 54 00:05 00:10 00:15 00:20 00:25 00:00:00 00:05:00 00:10:00 00:15:00 Time (minutes) Time (minutes) Turbidity probe:Turbidity percentage Turbidity probe:Turbidity percentage Reaction temperature:Temperature celsius Power supply: actual power Reaction temperature:Temperature celsius
Benefits of ultrasound-mediated crystallizations • Reduced induction time • Decreased Metastable Zone Width (MSZW) • Increased crystal growth rate • Reduced agglomeration • Tailored crystal size distribution • Polymorph control To overcome the issues associated with ultrasound probes (short lifetime due to cavitation/poor ultrasound energy distribution), Syrris offer the Atlas Sonolab.
Total crystallization control • Using proprietary ultrasound technology, the Sonolab allows fully automated control of: Particle size Shape Crystallinity Polymorphism • The Sonolab consists of an ultrasound flow cell and ultrasound generator • Unique flow cell designed to give uniform ultrasound radiation throughout, offering the highest levels of reproducibility/repeatability.
• Syrris offer two types of pressure vessel: - Atlas Sodium Pressure System (200 Bar) - Atlas Potassium Pressure System (3 Bar) • Designed for applications such as hydrogenations, carbonylations, catalyst screening etc. where elevated pressures are required. • Both systems are based on the Atlas Classic System, and are available with or without automation
Automating pressure reactions made easy Control manually or via PC for total reaction • control • Vessel range: 100, 160, 300 and 450 mL reactors available in SS, Hastelloy, titanium etc. Safety is assured with a pressure burst disc • and temperature cutouts • Pressure Control Module allows for precise pressure control and the Gas Selection Module allows selection of up to 3 gases.
3 Bar pressure up to 3 Litres • Tool-free pressure vessel changes allow vessels to be interchanged in minutes • Vessel sizes available: 100 mL, 250 mL, 500 mL, 1 L, 2 L or 3L • Accurately control temperature between -80 °C and +200 °C • To ensure safety, the Atlas 3 Bar system comes equipped with a pressure burst disc and pressure relief valve. • A safety enclosure is also provided for extra peace of mind.
Continue to Orb
A revolution in bench top reactors Designed with simplicity and flexibility in mind, Orb is the jacketed reactor system combining high performance and excellent value.
Simple click-lock system • No matter if you are using 100ml or 10L reactors , the simple click – lock system adjusts to ensure that you always have the perfect working height • All components and stirrer motor move together on the unique slide rail support • No other adjustment required.
Single handle to lift and swivel • Conveniently positioned handle to lift and swivel the stirrer motor for easy access to the reactor • No further adjustment required once the system is first installed, even when changing reactor sizes
Engineered for ease of use • Rapid action clamping mechanism • The unique patented clamp design allows opening without the risk of the glassware falling • Torque limited closure eliminates the risk of damage through overtightening
All the reactors you need in one compact footprint • Choice of 27 different reaction vessels 100 ml to 10 L , there is one for every application • Simple to operate , reconfigured to your needs in seconds • Robust heavy duty construction , engineered for years of service , day after day.
Continue to Orb Pilot
Products that you can trust Syrris has taken more that a 15 years to refine • its lab scale products. • The knowledge and experience gained by its engineers and scientists has been redirected to develop scale-up systems for both Batch and Flow chemistry • The same ethos of creative design, superior engineering and high performance has been carried forward into these new products
Orb Pilot is the ultimate scale-up batch reactor • Orb Pilot is the most flexible and easy to use batch reactor at this scale • Offering market leading performance at affordable prices High performance stirring Excellent thermal properties User friendly and clever features built in Wide variety of options and upgrades
High performance mixing is assured with a wide variety of impellor designs and powerful stirrer motors. Easy-fit Baffles are also offered in a selection of profiles to maximise the efficiency
stirring without baffles stirring with baffles
Orb Pilot reactors all feature a special oil inlet design which evenly distributes incoming oil around the base of the vessel ensuring uniform temperature around 360 O High performance, smooth bore, 20mm ID hoses ensure maximum oil flow.
Multiple working volumes in one footprint • Orb Pilot’s unique self -adjusting frame makes switching between vessels sizes a trivial exercise. • You can rapidly change between 10 L, 20 L, 30 L and 50 L reactors in a matter of minutes • Vacuum jacket vessels are available for ultra- low or high temperature applications
The combinations of easy-lift-and -swing motor mount, self adjusting frame and predefined clamp positions, make vessel changes very simple even for a novice user.
Industry standard designs and geometries • Stirrer options include industry standard A310 Hydrofoil impellors • Sizes and positions are optimised for the down-flow design ensuring the best possible mixing.
Continue to Chemisens
The most sophisticated reaction calorimetry system available • The unique design and measurement principle can provide data for processes where other systems struggle • The True Heat Flow principle allows precise and repeatable experiments at reflux, high pressure or during phase change with unrivalled sensitivity, accuracy and precision • Ideal choice for process development, kinetic studies, low-energy processes and reaction safety data generation
Design philosophy • Idea conceived and turned into product by Swedish researchers in polymer science in late 1980s • Syrris acquired the Chemisens company in 2015 to continue their ideas • Polymerizations are very challenging to measure using calorimeters – due to high changes in viscosity and/or phase changes • The unique design corrects for those phenomena, resulting in the most sensitive and sophisticated reaction calorimetry system available – not only for polymerizations!
True Heat Flow – the key for accurate measurements • Traditional methods suffer from shifting baseline – as a result of dosing/phase change – the data is always interpreted • Unique design of the reactor fights this – the heat exchange area – the base of the reactor - is always constant. It contains array of heat flow sensors, and Peltier element for temperature control • This principle enables the biggest feature of the system - stable zero baseline , even at reflux operation.
Ingenious design allows to run experiments unaffected by: • Different filling volumes • Reactor contents • Changes in viscosity • Changes in stirrer speed Stable zero baseline. No guessing. No interpreting. Precise and accurate real-time kinetic data All data can be logged (50 parameters, every 2 seconds) No calibration required – The heat transfer area is always the same
Thermograms of generic semi-batch reactions with CPA and HFC calorimeter. Thanks to this advantageous design, CPA measurements are very sensitive (± 0.01 W), and offers unrivalled performance accuracy, precision and sensitivity wise.
The standard system consists of: • Bench Unit Reactor with stirrer and reference thermostat • System Controller Processes all signals, connects to operator PC • PC ChemiCall V2 software suite CCReport V2 data manipulation software COMLI communication protocol • Dosing controller (Optional) Interface to connect various supporting devices Pumps, balances, sensors (pressure, pH etc.), valves Reflux condenser & reflux split kit
The heart of the system Volume of 250 mL, useful volume 10-180 mL • Lid fittings compatible with Swagelok system, • dosing ports available in base as well • Stirring 50-2000 rpm (10 Ncm) Temp ranges: -50 to +200 °C ( • HighSens: -20 to +150 °C 20 bar reactor available in SS316, HC276 and • Tantalum • 100 bar available in SS316 and HC276
The zero baseline allows for easy and precise operation at reflux. The reflux condenser measures heat dissipated using heat balance principle, and the signal is directly calculated in real-time in PC software.
Continue to Flow
• Flow chemistry is the process of performing chemical reactions in a continuous tube or pipe. A • Reagents are pumped together at a mixing C junction and the flow continues down a B temperature controlled tube or pipe. • The ratio of the reactants are controlled by their concentrations and relative flow rates. The rapid mixing and large surface area to volume ratio provides excellent reproducibility and control of a chemical process.
Skip flow principles
1. Residence Time 2. Mixing 3. Temperature 4. Pressure
Residence time is the time that every fraction of the reaction volume spends in the reactor, and is equivalent to reaction time in batch chemistry. Residence Time= Reactor Volume Total Flow Rate Two ways of controlling the residence time: • Vary the reactor volume. • Vary the flow rates. To control the molar ratio: • Vary the flow rates ratio
Residence Time= Reactor Volume Total Flow Rate Example: 2 reagents flowing into a 1 ml glass microreactor at 0.25 ml/min flow rate each. Combined flow rate = 0.25 + 0.25 = 0.5 ml/min Residence time = 1/0.5 = 2 min • What is the residence time? To change the residence time to 8 min. - Total Flow Rate Needed: 0.125ml/min (Each reagent with 0.0625 ml/min) OR • What are the two options? - Increase the reactor volume to 4 ml.
In batch chemistry, mixing is turbulent In flow chemistry, the mixing can be turbulent or laminar Small tube diameter results in laminar flow conditions (Reynolds number Re<2500) Radial diffusion
In turbulent flow conditions, static mixers are • used to increase mass transfer • In laminar flow conditions, mixing occurs by diffusion Diffusion time is proportional to distance squared, therefore over short distances, diffusion is fast and reproducible Reservoir Pump Reservoir Pump
Very high surface area to volume ratio • 100°C • Fast heat transfer: better temperature control Tr • Reactions cool down or heat up extremely rapidly (faster than a microwave) Small volume therefore flow reactors can be easily • pressurised • By pressurising, flow reactors can operate at temperatures above the typical boiling point of 100°C reactions This enables easy superheating of reactions e.g. 100ºC Tr to 150ºC above reflux temperatures at atmospheric pressure
Back pressure due to flow This increases with higher flow rate, narrower channels or more viscous liquid Reactions with gas – either adding gas into a reaction Back pressure intentionally applied or gas evolving reactions This is typically applied by a pressure regulator near Avoiding cavitation – volatile material boiling the exit of the system Superheating – taking material above its reflux temperature
Monophasic liquid-liquid reactions Biphasic liquid-liquid reactions Solid-liquid reactions Liquid-Gas Solid-Gas
• Reaction of CaCl 2 and Na 2 CO 3 to synthesize CaCO 3 in batch and flow • Exactly the same scale, concentration, temperature and reaction time • Quality and reproducibility clearly much higher in flow than batch Batch Flow
Homogeneous catalysis Ring formations General Synthesis • Suzuki reaction • Grubbs ring forming • Aldol reaction Heck reaction Ugi followed by ring Biphasic Schotten-Baumann • • • • Grubbs ring forming closure to • HBTU amide coupling benzimidazole Elimination of an alcohol to alkene • Multicomponent reactions Diels Alder Esterification of an alcohol • • • Passerini 3CR • 1,3,4 Oxadiazole • Wittig reaction Biginelli 3CR formation Nucleophilic aromatic substitution • • Ugi 4CR • Fischer indole synthesis • SN1 reaction • 1,3 Thiazole formation Mitsunobu reaction • • Deprotection chemistry Pyrazole formation N-Alkylation • • • BOC deprotection MOM deprotection and Oxidations and reductions Nanoparticles • intra epoxide opening • Borohydride reduction • Gold , Nickel, Silver, Iron (biosensors) • Ester saponification • Borane reduction of a heterocycle • Reductive amination Dess Martin alcohol • oxidation 85
The key benefits of flow chemistry are: • Faster reactions • Safer reactions • Faster reaction optimisation • Reaction conditions not possible in batch • Reactions are usually more selective • Easier scale-up • Simpler work-up • Easy integration of reaction analysis
It is much easier to pressurize flow reactors • Higher pressures enable higher temperatures • • Higher temperatures result in faster reaction rates
Poor selectivity comes from variations in • temperature, concentration and addition /stirring rates • Due to a high surface area:volume ratio and diffusion mixing, flow chemistry offers a much better parameters control. Potential energy E C A Reaction coordinate Excellent temperature control Minimal concentration gradient
• If a 10L batch reactor explodes, this has serious consequences • The same 10L can be passed through a 10ml flow reactor, ensuring that only 10ml is reacting at any time • For a fast reaction e.g. 1 min reaction this only takes an overnight run In this case the risk is 1/1000!!!
• Reaction time - Vary total flow rate • Reaction temperature - Low thermal mass • The ratio of reagents - Vary flow rate ratio • Concentration - Vary solvent stream One reaction is flushed out by the next (separated by a solvent) therefore only one reactor is used.
• Do you have a scale limit – COSHH ( Control • Do you have selectivity issues – can you of substances hazardous to health ), glassware control your stoichiometry etc. • Do you generate reactive intermediates or • Do you have a temp. limit – TSu, DSC, hazardous by-products cyrogenics, microwave • Do you have safety issues – see any of the • Do you require controlled addition – above exotherm’s, mixing, etc.
Syringe Pump Microreactor Pressure Product Collector Pumps are potentially the Flow chemistry reactors The ability to apply pressure Flow chemistry allows most important part of a need to cover the greatest to a flow chemistry reaction material to be collected flow chemistry system. range of reaction conditions. is a major benefit of using the without the restriction of Without confidence in Reactors should be flexible technique. Pressure allows reactor size. Small amounts pumping accuracy and in volume, provide excellent superheating of the reaction can be collected for reaction performance many of the mixing/heat transfer and mixture to increase reaction optimization and larger advantages of flow offer good visibility where rates and can also control quantities for scale up chemistry are lost. possible. reactions that evolve gas or applications. where gas is added as a reactant.
Asia is a revolutionary range of advanced • flow chemistry products from Syrris. It has been designed by chemists for chemists to enable the widest variety of chemical reactions and ultimate ease of use. The proprietary technology allows manually • controlled or fully automated experiments . • Asia offers maximum chemical resistance with an extensive range of temperatures, pressures, and reaction times on scales from mg to kg. • Asia celebrated its unique design as a winner of the R&D 100 Award for innovative technology.
Specifications • Reactor temperature: -100°C to +250°C • Liquid phase reactor volumes: 62.5 μ l, 250 μ l, 1ml, 4ml, 16ml • Solid phase reactor volumes: 0.7ml, 2.4ml, 5.6ml, 12ml • Pressure: 0 to 20bar (300psi) • Flow rate: 1μl/min to 10ml/min per pump channel • Residence times: 1 second to multi hour • Wetted materials: Glass, PTFE and PCTFE (stainless steel and hastelloy possible) • Mixing: Rapid diffusion mixing • Production volumes: micrograms to kilograms
• The Asia Starter Systems are ideal for chemists eager to begin using flow chemistry as well as academics interested in introducing flow chemistry to their group. • The easy-to-use and affordable system contain all essential flow system parts: an Asia Syringe Pump, an Asia Chip Climate Controller, a glass microreactor, and an Asia Pressure Controller. • The systems are future-proof and can be seamlessly upgraded with additional features and modules as the user experience with flow chemistry grows.
• The Asia Premium Flow Chemistry Systems offer a full range of Asia modules and enables standard flow chemistry operations as well as advanced use. • Ideal for chemists who are interested in the utmost functionality and access to the widest range of chemical space. • The Asia Premium Flow Chemistry Systems enables standard flow chemistry operations such as reaction optimization, scale-up, etc., as well as advanced flow chemistry such as electrochemistry, multi-step reactions, cryogenic reactions, etc.
Skip applications
Nitration of pyrazoles at AstraZeneca “In the case of a hazardous reaction, the risk of an incident is minimised as the accumulation of potentially dangerous intermediates is avoided.”
Continuous DIBAL-H reduction of a methyl ester in flow. Garner´s Aldehyde: Chiral starting material for natural • product synthesis – used in over 100 natural product synthesis (very expensive) • Reaction requires immediate quenching of the DIBAL reagent to prevent further reduction. Batch: difficult to control direct transformation . • ester 1° step - reduction 2° step - oxidation DIBAL – H common reducing agent Difficult to handle: air moisture sensitive, pyrophoric. Continuous Flow-Processing of Organometallic Reagents , Duncan Browne, Steve V. Ley OPRD, 2015.
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