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Efficient solution-phase protocols for the high-throughput synthesis of 6-(1,2,3-triazol-1-yl)-dihydropyrimidones are reported. The multistep sequence involves the initial bromination of dihydropyrimidones precursors (DHPMs, Biginelli compounds) at the C6-methyl position, using a recyclable polymer-supported brominating agent under rapid flow-through conditions (residence time of 1 min). The 6-bromomethyldihydropyrimidone intermediates were subsequently subjected to a microwave-assisted azidation step (25 min), providing the key 6-azidomethyldihydropyrimidone precursors. In the final step of the sequence, the azides were treated with terminal acetylenes under Cu(I) catalysis (azide-acetylene ligation, "click chemistry") to provide the target 6-(1,2,3-triazol-1-yl)-dihydropyrimidones in a regiospecific fashion (1,4-triazoles) in moderate overall yield utilizing controlled microwave irradiation (20 min). In total, a library of 27 compounds was prepared with 4 points of diversity. 相似文献
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Different scavenging techniques using polymer-supported sequestration agents are described for the purification steps in the synthesis of N3-acylated dihydropyrimidines. For scavenging both excess anhydride and unwanted byproducts, polystyrene and silica supported diamines, aminomethyl-functionalized SynPhase Lanterns and diethylenetriamine StratoSpheres Plugs are used. In both synthesis and purification microwave flash heating was utilized, reducing reaction times from hours to minutes. These two steps coupled with an efficient solid-phase extraction (SPE) workup allowed the generation of a 28-member library of N3-acylated dihydropyrimidines using anhydrides. Using related protocols a 15-member library of N3-functionalized dihydropyrimidines utilizing acid chlorides as acylating reagents was also obtained. 相似文献
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Damm M Holzer M Radspieler G Marsche G Kappe CO 《Journal of chromatography. A》2010,1217(50):7826-7832
An efficient microwave-assisted high-throughput protein hydrolysis protocol was developed utilizing strongly microwave absorbing silicon carbide-based microtiter platforms. The plates are equipped with 20 bore holes having the proper dimensions for holding standard screw-capped HPLC/GC vials. Due to the possibility of heating up to four heating platforms simultaneously (80 vials), parallel microwave-assisted acid hydrolyses can be performed under carefully controlled conditions significantly reducing the overall time required for protein hydrolysis and the subsequent evaporation step required for larger volumes of acid. An extensive optimization of the hydrolysis conditions has demonstrated that 5min irradiation at 160°C with 6N HCl leads to comparable results in terms of total and individual amino acid recovery as the traditional method requiring 24h heating at 110°C. Complete hydrolysis of several proteins and synthetic peptides was performed using 25μg of sample material and 100μL of 6N HCl in a dedicated low-volume HPLC/GC vial. Since the hydrolysis and subsequent analysis can be performed from the same vial, errors caused by sample transfer can be minimized. Control experiments have demonstrated that the observed rate enhancements are the result of a purely thermal/kinetic effect as a consequence of the considerable higher reaction temperatures. 相似文献
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T.?RublackEmail author S.?Hartnauer P.?Kappe C.?Swiatkowski G.?Seifert 《Applied Physics A: Materials Science & Processing》2011,103(1):43-50
The selective ablation of thin (∼100 nm) SiO2 layers from silicon wafers has been investigated by applying ultra-short laser pulses at a wavelength of 800 nm with pulse
durations in the range from 50 to 2000 fs. We found a strong, monotonic decrease of the laser fluence needed for complete
ablation of the dielectric layer with decreasing pulse duration. The threshold fluence for 100% ablation probability decreased
from 750 mJ/cm2 at 2 ps to 480 mJ/cm2 at 50 fs. Significant corruption of the opened Si surface has been observed above ∼1200 mJ/cm2, independent of pulse duration. By a detailed analysis of the experimental series the values for melting and breaking thresholds
are obtained; the physical mechanisms responsible for the significant dependence on the laser pulse duration are discussed. 相似文献
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