An efficient ESI-MS(n) method for the structural identification and isomeric differentiation of flavonol O-rhamnosides was developed. The differences in the glycosyl type, and the glycosylation and methoxylation positions in the structures of isomeric flavonoids, can be determined using (-)ESI-MS(n) spectra. The formation and relative abundances of [Y(0)-H](-•) and Y(0) (-) ions, as well as the comparison of some diagnostic ions, are vital in the differentiation of isomeric flavonoids. These results have practical applications in the rapid identification of flavonol O-rhamnosides present in crude bioactive extracts.
A series of novel 5-amino-7-aryl-7,8-dihydro-[1,2,4] triazolo[4,3-a]-pyrimidine-6-carbonitriles were synthesized by a one-pot reaction of 3-amino-1,2,4-triazole, malononitrile and aryl aldehydes in the presence of 20 mol% NaOH in ethanol under heating or ultrasonic irradiation. The structures of the target compounds were confirmed by inspection of their 1H- NMR, 13C-NMR, IR and MS spectra. The advantages of this method are short reaction times, good yields, high selectivity and operational simplicity.
A series of 6-amino-4-aryl-3-methyl-2,4-dihydropyrano[2,3-c]pyrazole-5-carbonitriles (5a-5j) were synthesized by four-component one-pot reaction of methyl acetoacetate (or ethyl acetoacetate), hydrazine hydrate, arylaldehydes and malononitrile in the presence of phase transfer catalyst. A highest yield of product was obtained while using 30 mol % of HDBAC as a catalyst.
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