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The reactions under microwave heating were carried out in a Smith Creator, part of Coherent Synthesis™ from Personal Chemistry. The used system operated with an emission frequency of 2.45 GHz and a reactor with on-line temperature, pressure and microwave power control. In this apparatus, reactions can be performed at any temperature in the range of 60 to 250°C at pressures of up to 2 MPa (20 bar). The temperature increase can be varied in the range 2-5°C/s, depending on the solvent. The reactions are performed under magnetic stirring, in vials with caps supplied by Personal Chemistry. The instrument processes reaction volumes between 0.5 and 5 mL.
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27
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33644766104
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note
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Initially, the reactions were monitored by NMR spectroscopy on aliquots of the crude reaction mixtures, taken from the vials with a syringe.
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28
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4544307133
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One of the referees of this article criticized our calling this a "three-component reaction", but we really cannot see the difference between our reaction and the well-known Ugi multi-component reactions in which, according to Ugi's own statement "the starting materials do not react simultaneously in one step, but rather in a sequence of elementary steps, according to a program." See: A. Dömling, I. Ugi, Angew. Chem. 2000, 112, 3300-3344;
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