高效液相色谱纯化技术：不对称硫代巴比妥酸的合成

HPLC purification technique: synthesis of unsymmetrical thiobarbituric acids.

作者信息

Deotale Vinod D, Katiya Manish M, Dhonde Madhukar G

机构信息

Department of Chemistry, Shri Mathuradas Mohota College of Science, Nagpur, 444009, MS, India.

出版信息

Heliyon. 2019 Jul 25;5(7):e02008. doi: 10.1016/j.heliyon.2019.e02008. eCollection 2019 Jul.

DOI:10.1016/j.heliyon.2019.e02008

PMID:31384677

原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC6664147/

Abstract

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 -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.

摘要

据报道，在乙酰氯 - 乙酸介质中，1,3 - 二取代硫脲与丙二酸反应合成硫代巴比妥酸；在室温搅拌下，1-(2 - 羟乙基)-芳基硫脲与丙二酸在对甲苯磺酸、乙酰氯 - 乙酸介质中相互作用合成环化嘧啶 - 7 - 酮。本方法是现有方法的高度环保替代方案，减少了乙酰氯的过量使用，并且借助反相高效液相色谱在254 nm处用光电二极管阵列（PDA）检测，通过1H、13C NMR和MS光谱进行光谱表征，对所有合成分子的纯度进行了检测。