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HPLC purification technique: synthesis of unsymmetrical thiobarbituric acids

Synthesis of thiobarbituric acids by the reaction of 1,3-disubstituted thioureas and malonic acid in acetyl chloride-acetic acid medium and synthesis of cyclized pyrimidin-7-one by the interaction of 1-(2-hydroxyethyl)-aryl thioureas, with malonic acid in p-tolyl sulphonic acid and acetyl chloride-a...

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Detalles Bibliográficos
Autores principales: Deotale, Vinod D., Katiya, Manish M., Dhonde, Madhukar G.
Formato: Online Artículo Texto
Lenguaje:English
Publicado: Elsevier 2019
Materias:
Acceso en línea:https://www.ncbi.nlm.nih.gov/pmc/articles/PMC6664147/
https://www.ncbi.nlm.nih.gov/pubmed/31384677
http://dx.doi.org/10.1016/j.heliyon.2019.e02008
Descripción
Sumario:Synthesis of thiobarbituric acids by the reaction of 1,3-disubstituted thioureas and malonic acid in acetyl chloride-acetic acid medium and synthesis of cyclized pyrimidin-7-one by the interaction of 1-(2-hydroxyethyl)-aryl thioureas, with malonic acid in p-tolyl sulphonic acid and acetyl chloride-acetic acid medium at room temperature stirring has been reported. The present protocol is highly eco-friendly alternative to existing methods, reduces the excess use of acetyl chloride and purity of all synthesized molecules checked with the help of reverse phase high performance liquid chromatography with photo diode array (PDA) detection at 254 nm with spectral characterization by 1H, 13C NMR, and MS spectra.