Raheem Abbasriyaludeen Abdul, Thangasamy Pitchai, Sathish Marappan, Praveen Chandrasekar
Materials Electrochemistry Division, Central Electrochemical Research Institute (CSIR Laboratory) Alagappapuram Karaikudi-630003 Tamil Nadu India
Academy of Scientific and Innovative Research (AcSIR) Ghaziabad-201002 Uttar Pradesh India.
Nanoscale Adv. 2019 Jun 27;1(8):3177-3191. doi: 10.1039/c9na00240e. eCollection 2019 Aug 6.
Preparation of gold nanoparticles (AuNPs) in environmentally friendly water without using any reducing agents under supercritical conditions is demonstrated. PXRD, XPS, FE-SEM and HR-TEM analysis confirmed the formation of phase-pure and crystalline AuNPs of the size of ∼10-30 nm. The catalytic potential of AuNPs was manifested through a generalized green procedure that could accommodate both Sonogashira as well as Suzuki coupling under aqueous conditions at low catalytic loading (0.1 mol%). The AuNP catalyst was found to be recuperated after the reaction and reused for up to six catalytic cycles with no leaching out of gold species as confirmed through ICP-OES analysis. With no confinement of AuNP catalysis to cross-coupling reaction, synthetic extension to one-flask preparation of π-conjugated semiconductors (4 examples) and their optoelectronic properties were also investigated. Other significant features of the present work include short reaction time, site-selectivity, wide substrate scope, high conversion, good chemical yields and applicability in gram-scale synthesis. Overall, the results of this paper signify an operationally sustainable supercritical fluid processing method for the synthesis of AuNPs and their catalytic application towards cross-coupling reactions in green media.
本文展示了在超临界条件下,无需使用任何还原剂,在环境友好型水中制备金纳米颗粒(AuNPs)的方法。粉末X射线衍射(PXRD)、X射线光电子能谱(XPS)、场发射扫描电子显微镜(FE-SEM)和高分辨透射电子显微镜(HR-TEM)分析证实,形成了尺寸约为10 - 30 nm的纯相且结晶的AuNPs。AuNPs的催化潜力通过一种通用的绿色方法得以体现,该方法能够在低催化负载量(0.1 mol%)的水性条件下,实现Sonogashira偶联反应以及Suzuki偶联反应。通过电感耦合等离子体发射光谱(ICP-OES)分析证实,AuNP催化剂在反应后能够回收,并可重复使用多达六个催化循环,且没有金物种浸出。由于AuNP催化不限于交叉偶联反应,因此还研究了其在一锅法制备π共轭半导体(4个实例)方面的合成扩展及其光电性质。本工作的其他显著特点包括反应时间短、位点选择性、底物范围广、转化率高、化学产率良好以及在克级合成中的适用性。总体而言,本文的结果表明了一种在操作上可持续的超临界流体处理方法,用于合成AuNPs及其在绿色介质中对交叉偶联反应的催化应用。