Summary: | Triazolo[4,3-<i>a</i>]pyrimidine is one of the promising structural fragments for the development of drugs, including anticancer drugs. This work is devoted to the synthesis of a number of new 2-arylhydrazone derivatives of thiazolo[3,2-<i>a</i>]pyrimidine, which are synthetic precursors for triazolo[4,3-<i>a</i>]pyrimidines. The crystal structure of 6-acetyl-7-methyl-5-phenyl-2-(2-phenylhydrazineylidene)-5<i>H</i>-thiazolo[3,2-<i>a</i>]pyrimidin-3(2<i>H</i>)-one was established by SCXRD. In the reduction reaction of the compound, the following system was used: vanadium(V) oxide, and sodium borohydride in ethanol at room temperature, which led to the formation of only one pair of diastereomers (1<i>R*</i>)-1-((5<i>S*</i>,6<i>R*</i>,7<i>R*</i>)-(1-(hydroxymethyl)-7-methyl-1,5-diphenyl-1,5,6,7-tetrahydro[1,2,4]triazolo[4,3-<i>a</i>]pyrimidin-6-yl)ethan-1-ol.
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