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Cleaning Microreactors
Syrris Ltd
This application note gives hints and tips on cleaning & unblocking flow reactors, i.e. chips or tube based reactors. It is suggested that the whole document is read before attempting to unblock a reactor.
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The Basics of Flow Chemistry
Syrris Ltd
This application note gives information on the basics of flow chemistry, with particular reference to the FRX system.
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Examples of FRX Applications for Demonstration
Syrris Ltd
FRX as a product offers a wide range of applications in a number of areas. To try and increase the exposure of the product to a wider audience, two standard demonstrations are detailed here. The first is a Wittig reaction showing the operation of an FRX200 system. The second is a separation of water and ethyl acetate demonstrating the operation of the FLLEX (Flow Liquid Liquid EXtraction module), for FRX300 or FRX400.
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Planning Successful Reactions
Syrris Ltd
This application note gives hints and tips for planning successful FRX reactions.
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Superheating Reactions
Syrris Ltd
When using the Pressurisation Module, the FRX system can be easily pressurised up to 7bar. This allows reactions to be performed at temperatures much higher than atmospheric reflux, enabling faster and often cleaner, higher yielding reactions. This application note describes the practicalities of superheating reactions and the suggested maximum temperatures for common solvents.
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Reaction Optimisation and Large Scale Synthesis
Syrris Ltd
A major benefit of flow chemistry is the ease and consistency of reaction scale up. In a flow reactor, high quality, reproducible mixing, excellent temperature control and superheating are maintained when increasing reaction volume.
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Analysis of Baculovirus in media on deltaDOT’s CE platform
deltaDOT
Here we describe a rapid, highly quantitative method used to analyse Baculovirus in growth media that is also applicable for real time monitoring of viral growth. Reproducibility by migration time was shown to be <0.6%.The current analytical techniques for the analysis of virus concentration in growth media is time consuming (24hrs minimum), labour intensive and has limited value for quantitation.
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Analysis of E.coli lysate using Peregrine High Performance Capillary Electrophoresis (HPCE) with Label Free Intrinsic Imaging (LFII™)
deltaDOT
Analytical instruments with the capability of analyzing complex mixture of bio-molecules with high precision, excellent reproducibility and quantitative indications are highly sought after in fields ranging from routine quality control procedure in bio-molecule production to biomarker discovery and diagnostic industry. This application note describes the high resolution separation and subsequent molecular weight characterization of four of the most abundant protein in E. coli cell lysate, using
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The Basics Of Flow Chemistry
Syrris Ltd
This application note gives information on the basics of flow chemistry, with particular reference to the Africa system.
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Planning Successful Reactions
Syrris Ltd
This application note gives hints and tips for planning successful Africa reactions.
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Cleaning Flow Reactors
Syrris Ltd
This application note gives hints and tips on cleaning & unblocking Africa flow reactors, i.e. chips or tube reactors.
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Examples of Africa Chemistry
Syrris Ltd
This application note describes examples of some of the chemistry performed using the Africa system. This is not intended to be a detailed analysis of each reaction, more a demonstration of the range of reactions possible.
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Reaction Optimisation 1
Syrris Ltd
This application note describes the optimisation of a Passerini reaction. The objective was to optimise a literature procedure to reach the highest yield of desired product with a maximum of 1hr reaction time.
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Reaction Optimisation 2
Syrris Ltd
This application note describes the optimisation of 2 out of 4 substitution reactions given to Syrris by a pharmaceutical company. The pharma company in question had attempted some reaction optimisation by traditional techniques but always had starting material remaining, even after a week long reaction. The starting materials (of commercial sensitivity) were given to Syrris with the objective of using the Africa synthesis & analysis system to optimise to 100% conversion.
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Superheating Reactions
Syrris Ltd
When using the Pressurisation Module, the Africa system can be easily pressurised up to 7bar. This allows reactions to be performed at temperatures much higher than atmospheric reflux, enabling faster and often cleaner, higher yielding reactions. This application note describes the practicalities of superheating reactions and the suggested maximum temperatures for common solvents.
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Reactor Size Selection
Syrris Ltd
One of the key differences between batch and flow is that for flow reactions, residence time, reactor volume and throughput are all linked. Therefore increasing the volume of the reactor will increase the residence time (if the flow rate is kept constant) or increase the flow rate (if the residence time is kept constant). This document gives information on how to select the right reactor for the right application.
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Africa and Design of Experiments
Syrris Ltd
Reaction optimisation work using traditional techniques can be complex, time consuming and expensive, but is a vital part of the development of all chemical processes. One approach is the use of statistical experimental design (DoE). This application note gives some guidance on DoE and it’s use with the Africa system.
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Flow Aqueous Work-up Using FLLEX
Syrris Ltd
This application note demonstrates the use of the Africa FLLEX (Flow Liquid Liquid EXtraction) module for performing post reaction automated liquid-liquid extraction in a standard Africa flow system. An amide coupling reaction was performed in the Africa system and worked up by extraction with aqueous bicarbonate to remove by-products. The quality of extraction and separation was the same batch.
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Biphasic Reactions
Syrris Ltd
A biphasic reaction involving electrophilic substitution of orcinol with a diazonium salt has been examined in the Africa flow system. The two-phase product solution was separated in the FLLEX module to give the azo product in the organic stream and an aqueous waste stream.
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The Mono-Boc protection of p-xylylenediamine in the Africa flow microreactor
Syrris Ltd
Microreactors offer rapid chemical optimisation coupled with minimal use of starting materials. The experiment described, vide infra, is part of a one day investigation into the synthesis optimisation of N-Boc-p-xylylenediamine.
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The Forced Degradation (De-esterification) of Parabens Using a Microreactor Flow System
Syrris Ltd
Product degradation studies are an important test for any pharmaceutical or other high value active material. These experiments generally expose the material to an external stress to assess the stability of the constituents or formulation. External stresses may include temperature, pH, light, moisture, and even exposure to other materials within the product formulation, and their degradation products.
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The Importance of Mass Transfer in Gas-Liquid Reactions
Chemspeed
Mass transfer can be a limiting factor in many industrially important gas-liquid phase reactions, such as hydrogenation and hydroformylation. Volumetric gasliquid mass transfer coefficients (klv) are used to assess the efficiency of mass transfer in different reactor types. In this study klv values have been determined for Chemspeed’s 13 mL and 100 mL synthesizer glass reactors, employing vortex agitation, and these results are compared with those for 2 other reactor types.
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Increased Efficiency in Chemical Process R&D: The Discovery of an Innovative One-Step Synthesis of Tetronic Acid
Chemspeed
Tetronic acid is an important key intermediate for different products (e.g. (+)-Biotin and Losigamon) of the fine chemical and pharmaceutical industry. Industrial production of tetronic acid is achieved in a multi-step process, starting from 4-chloro acetoacetate. It was found, that addition of 4-chloro acetoacetate to a cold, aqueous solution of sodium hydroxide yields a mixture of sodium chloroacetate and sodium acetate. In addition, the resulting yield of sodium tetronate is less than 30%.
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Chemspeed‘s MiniPlant for Specialty Gases Chemistry: Controlled Feeding of Specialty Gases
Chemspeed
The scope of Chemspeed’s MiniPlant technology allows the controlled feeding of specialty gases against pressure. Liquefied gases such as alkylene oxides and isobutylene have been successfully applied for corresponding polymerization and alkylation chemistry, respectively. Highly hazardous and reactive gaseous monomers have been successfully applied in polymerization under pressure of a three-component (two monomer mixtures and one reactive gas) mixture.
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On-Line Reaction Monitoring by FT-NIR - The Formation of Tetronic Acid Sodium Salt from 4-Chloro Acetoacetate
Chemspeed
4-Chloroacetoacetate in aqueous media cyclizes in highchemical yields to tetronic acid sodium salt , when this transformation is carried out under very careful and tight control of the critical reaction parameter (temperature and pH).Competing with this process, and depending on the control of these reaction parameters, a retro Claissen reaction might be observed as the main process which cleaves 4-chloroacetoacetate to yield a mixture of sodium acetate and sodium chloroacetate.
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