High-throughput experimentation

About 10 years after the application of combinatorial methods to organic chemistry, especially in the development of new drugs in the pharmaceutical industry, combinatorial and high-throughput methods were also applied in 

Synthesis of Solid Catalysts. Edited by K.P. de Jong 2009 WILEY-VCH Verlag GmbH Co. KGaA, Weinheim ISBN 97S-3-527-32040-0 

Tabie 11.1 Comparison of stage I and stage I high-throughput catalysis. 

Integration Very high (100-10 000 experiments/day) Moderate (10-100 experiments/day) 

Preparation Methods adapted from inorganic materials preparation, spots on wafer substrates, ig amounts of powder Methods adapted from lab or industrial preparation (impregnation, precipitation, crystallization, calcination, reduction), 0.5-20 g 

Composition type Process variables Analysis methods  

Polymorphs and solvates Salts and co-crystals Thermal Evaporation Anti-solvent Slurry conversion Other variables In situ HT Ex situ LT 

Solvent type Counter-ion Heating rate Rate of Anti-solvent Solvent type Mixing rate Optical DSC 

Degree of Cooling rate Incubation Impeller design copy TGA 

Additive con- tempera- anti-solvent Thermal etc.) FTIR Single 

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The constantly increasing amount of data coming from high throughput experimental methods, from genome sequences, from functional- and structural genomics has given a rise to a need for computer-assisted methods to elucidate sequence-structure-function relationships. 

Active heterogeneous catalysts have been obtained. Examples include titania-, vanadia-, silica-, and ceria-based catalysts. A survey of catalytic materials prepared in flames can be found in [20]. Recent advances include nanocrystalline Ti02 [24], one-step synthesis of noble metal Ti02 [25], Ru-doped cobalt-zirconia [26], vanadia-titania [27], Rh-Al203 for chemoselective hydrogenations [28], and alumina-supported noble metal particles via high-throughput experimentation [29]. 

Zech, T, Schunk, S., Klein, J., Demuth, D., The integrated materials chip for high-throughput experimentation in catalysis research, in Proceedings of the 6th International Conference on Microreaction Technology, IMRET 6, pp. 32-36 (11-14 March 2002), AIChE Pub. No. 164, New Orleans. 

H.-J., Lowe, H., de Belleeon, C., Pestre, N., Lamouille, T., Grenouillet, P., High-throughput experimentation with a micromixer based, automated serial... 

HTE High-throughput experimentation iPIXE Imaging particle-induced X-ray... 

DESIGN OF EXPERIMENTS COMBINED WITH HIGH-THROUGHPUT EXPERIMENTATION FOR THE OPTIMIZATION OF DeNO CATALYSTS... 

High-throughput experimentation (HTE) has attracted much (and not always positive. ..) attention in the scientific and industrial communities in the past few years [1-3]. 

HIGH-THROUGHPUT EXPERIMENTAL SETUP AND DATA ANALYSIS... 

Dar, Y.L. (2004) High-throughput experimentation a powerful enabling technology for the chemicals and materials industry. Macromol. Rapid Commun., 25, 34. 

Al-Saeedi, J.N. and Guliants, V.V. (2002) High-throughput experimentation in multicomponent bulk mixed metal oxides Mo-V-Sb-Nb-O system for selective oxidation of propane to acrylic acid. Appl. Catal. A Gen, 237, 111. 

Kubanek, P., Busch, O., Thomson, S. et al. (2004) Imaging reflection IR spectroscopy as a tool to achieve higher integration for high-throughput experimentation in catalysis research. J. Comb. Chem., 6, 420. 

Hendershot, R.J. (2004) Statitically Guided High-Throughput Experimentation of NOx storage and Reduction. Doctoral Thesis, Morris Library, University of Delaware. 

Hendershot, R.J., Rogers, W.B., Snively, C.M. et al. (2004) Development and optimization of nox storage and reduction catalysts using statistically guided high-throughput experimentation. Catal. Today, 98, 375. 

HTE high-throughput experimentation TOF turnover frequency TON turnover number... 

Immobilized catalysts on solid supports inherently have benefits because of their easy separation from the products and the possibility of recycling. They are also expected to be useful for combinatorial chemistry and high-throughput experimentation. The polystyrene-bound BINAP/DPEN-Ru complex (beads) in the presence of (CH3)3COK catalyzes the hydrogenation of l -acetonaphthone with an SCR of 12 300 in a 2-propanol-DMF mixture (1 1, v/v) to afford the chiral alcohol in 97% ee (Fig. 32.35) [113]. This supported complex is separable... 

In conclusion, it seems likely that high-throughput experimentation (HTE) will not only be a tremendous methodology to solve the time-to-market problem, but will also enhance the scope as well as the quality of academic research to a large extent. 

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