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High-performance thin-layer chromatography has been used to follow the synthesis of some quinoxalinone derivatives by biocatalysis in a one-pot reaction, as an alternative route to the poor Hinsberg reaction. The progress of the one-pot reactions can be followed by HPTLC without previous isolation of the different intermediates arising from them. Biocatalytic synthesis of quinoxalinone derivatives leads to an irreversible reaction which gives a single product of high purity and yields in excess of 90–95%.
Abstract
A facile and benign route to N-heterocycles, including triazoles and triazolopyrimidines, has been developed. Using continuous-flow microreactor technology, organic azides are prepared in situ and reacted with cyanoacetamide in a [3+2] cycloaddition to produce a variety of substituted 1,2,3-triazoles, which can be elaborated into useful building blocks. A benzyl-substituted triazole was further functionalized to an analog of the core structure of the antiplatelet agent Brilinta®. The methodology lends itself well to flow chemistry, where reaction volumes are minimized, heating and mixing are consistent, and the need for intermediate azide isolation bypassed. The scope of the process is wide, and the efficiency is high, suggesting this as a practical, green route for the production of triazolo-based heterocycles.
Abstract
A series of changes and updatings to the [18F]FDG setup of the Anatech RB-86 robotic system are described. They include improved [18O]H2O recovery, “one-pot” reaction, elimination of the SPE step and base-assisted hydrolysis. Considerations on this last point are also reported. Thus, a remarkable improvement in the radiochemical yield, which is now 81% (decay corrected to SOS) with a synthesis time of just 40 minutes, has been achieved. The influence of several different reaction vessel materials on the synthesis is also briefly examined.
( n -C 4 H 9 ) 4 [Fe II Fe III (C 2 O 4 ) 3 ]} ∞ (Scheme 1 ) and attempt to identify the reaction processes. Experimental The precursor material {N( n -C 4 H 9 ) 4 [Fe II Fe III (C 2 O 4 ) 3 ]} ∞ was prepared in one pot
. Results and discussions Synthesis and physico-chemical characterisation of complexes The one-pot reactions of excess formaldehyde with 2:2:1 molar mixture of nickel(II), copper(II) or zinc (II) chloride, 3,6-diazaoctane-1
Synthesis and physico-chemical characterisation of complexes and ligand The one-pot reactions of excess formaldehyde with 2:2:1 molar ratio of nickel (II), copper(II) or zinc (II) acetate, 3,6-diazaoctane-1,8-diamine and 1,2-phenylenediamine in an
