Small-Scale Synthesis of Laboratory Reagents with Reaction Modeling

Lerner, Leonid

doi:10.1201/b10611

Cited by 8 publications

(9 citation statements)

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“…The ease of manual handling and the dimensions of the reaction flasks used in standard laboratories define the practical lower limit range to millilitres and hundreds of milligrams of substances (without utilizing additional specialized equipment). Indeed, even small‐scale syntheses are often calibrated not due to a need for such quantities of material but as a consequence of human handling and convenience . This can mean that over long synthetic sequences large quantities of starting materials are required in order to elaborate the structures (loss of material through incomplete reaction, by‐product formation or manual intervention).…”

Section: Our Current Synthesis Capabilitymentioning

confidence: 99%

“…Indeed, even small-scale syntheses are often calibrated not due to a need for such quantities of material but as a consequence of human handling and convenience. 21 This can mean that over long synthetic sequences large quantities of starting materials are required in order to elaborate the structures (loss of material through incomplete reaction, by-product formation or manual intervention). Furthermore, testing and optimizing the required synthetic steps involves a significant investment of time and manpower as well as precious substrates/reagents.…”

Section: Our Current Synthesis Capabilitymentioning

confidence: 99%

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The integration of flow reactors into synthetic organic chemistry

Baxendale

2013

J of Chemical Tech & Biotech

242

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The material presented in this review is based upon discussions and interactions with members of the Department of Chemistry and Biochemistry within the University of Windsor, Ontario, Canada. This article explores the changing face of chemical synthesis with regard to the impact of flow based chemical processing technologies. Highlighted works from the Innovative Technology Centre (ITC), Cambridge, UK, are used to illustrate the alternative synthetic practices available to modern research chemists. The dominant theme of the review is the synergistic effects encountered by combining the advantages of continuous processing regimes with the power of immobilized reagents and scavenger systems for multi‐step organic chemistry. © 2012 Society of Chemical Industry

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Section: Our Current Synthesis Capabilitymentioning

confidence: 99%

Section: Our Current Synthesis Capabilitymentioning

confidence: 99%

The integration of flow reactors into synthetic organic chemistry

Baxendale

2013

J of Chemical Tech & Biotech

242

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“…CCD at 3 levels, 2 factors was selected as independent variables and the interaction of variables were estimated. 9 runs were carried out to fit the general model of equation (1) and to obtain economically optimum conditions for the SO3 removal efficiency.…”

Section: Experimental Designmentioning

confidence: 99%

“…Sulphur trioxide is invisible odourless but corrosive gas which is considered as an environmental pollutant [1,2]. It can be produced in an industrial scale as a precursor to sulphuric acid which has numerous industrial applications.…”

Section: Introductionmentioning

confidence: 99%

Prediction and Optimization of Sulphur Trioxide Yield from Calcination of Aluminium Sulfate Using Central Composite Design

Olubajo

Makarfi

2019

PoS

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Sulphur trioxides are common toxic gaseous pollutants which can be produced from alternative routes via calcination of aluminum sulfate derived from kaolin clay. Its demand increases geometrically, thus the need to optimize the yield of SO 3 from the calcination of alum is essential. The rate of alum decomposition was monitored by the formation of SO 3 via thermogravimetric analysis and X-ray fluorescence analysis. This study aimed to evaluate the effect of calcination temperature and curing time on the SO 3 conversion and yields using Face Central Composite Design and optimize the process conditions to evaluate the maximum yield of SO 3 using response surface methodology and its effects and interactions were investigated between 800-900 °C at 60-180 minutes. Results indicated that experimental data satisfied second order polynomial regression model for SO 3 conversion and SO 3 yield from TG analysis while XRF analysis satisfied first order model respectively. An increase in SO 3 conversion and yields was observed as the calcination temperature and time were increased both independently and simultaneously. The calcination temperature was found to have a stronger influence compared to the calcination time. Validation indicated agreement between experimental and predicted values with a regression value of 97.8 %, 97.77 % and 97.67 % for SO 3 conversion, SO 3 yield via TG and XRF analyses respectively. Based on the ANOVA, the SO 3 yield via XRF produced the best model with R 2 pred of 91.98% while SO 3 yield via TG analysis and SO 3 conversion had R 2 pred of 79.99% and 78.01% respectively. Optimization of the production of SO 3 was carried out and the optimal condition for SO 3 conversion, SO 3 yield via TG and XRF analyes were 90.11 %, 91.67 % and 75.81 % respectively at an optimal calcination temperature of 877.43 o C and time of 155.04 minutes respectively.

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“…Phenyl azide was discovered by Griess in 1864 by diazotization of phenyl hydrazine with nitrous acid [1] and in 1890, Curtius, using hydrazine and nitrous acid, discovered hydrazoic acid under an identical diazotization approach [2]. At that time, sodium azide and potassium azide were also obtained from hydrazine and an alkyl nitrite respectively in NaOH or KOH [3].…”

Section: Introductionmentioning

confidence: 99%

Azides and Porphyrinoids: Synthetic Approaches and Applications. Part 1—Azides, Porphyrins and Corroles

et al. 2020

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Azides and porphyrinoids (such as porphyrin and corrole macrocycles) can give rise to new derivatives with significant biological properties and as new materials’ components. Significant synthetic approaches have been studied. A wide range of products (e.g., microporous organic networks, rotaxane and dendritic motifs, dendrimers as liquid crystals, as blood substitutes for transfusions and many others) can now be available and used for several medicinal and industrial purposes.

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Small-Scale Synthesis of Laboratory Reagents with Reaction Modeling

Cited by 8 publications

References 0 publications

The integration of flow reactors into synthetic organic chemistry

The integration of flow reactors into synthetic organic chemistry

Prediction and Optimization of Sulphur Trioxide Yield from Calcination of Aluminium Sulfate Using Central Composite Design

Azides and Porphyrinoids: Synthetic Approaches and Applications. Part 1—Azides, Porphyrins and Corroles

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