ZnCl2 loaded TiO2 nanomaterial: an efficient green catalyst to one-pot solvent-free synthesis of propargylamines

被引：14

作者：

Bankar, Digambar B. ^{[1
,2
]}

Hawaldar, Ranjit R. ^{[1
]}

Arbuj, Sudhir S. ^{[1
]}

Moulavi, Mansur H. ^{[1
]}

Shinde, Santosh T. ^{[4
]}

Takle, Shrikant P. ^{[1
]}

Shinde, Manish D. ^{[1
]}

Amalnerkar, Dinesh P. ^{[3
]}

Kanade, Kaluram G. ^{[1
,3
]}

机构：

[1] C MET, Off Pashan Rd, Pune 411008, Maharashtra, India

[2] RB Narayanrao Borawake Coll, PG Dept Chem, Shrirampur 413709, Ahmednagar, India

[3] Yashavantrao Chavan Inst Sci, PG & Res Ctr, Satara 415001, India

[4] Annasaheb Awate Coll, PG Dept Chem, Pune 410503, Maharashtra, India

来源：

RSC ADVANCES | 2019年 / 9卷 / 56期

关键词：

C-H ACTIVATION; 3-COMPONENT SYNTHESIS; COUPLING REACTIONS; MULTICOMPONENT SYNTHESIS; A(3)-COUPLING REACTION; RECYCLABLE CATALYST; CRYSTAL-STRUCTURES; REUSABLE CATALYST; TERMINAL ALKYNES; SECONDARY-AMINES;

D O I：

10.1039/c9ra06693d

中图分类号：

O6 [化学];

学科分类号：

0703 ;

摘要：

One-pot green synthesis of propargylamines using ZnCl2 loaded TiO2 nanomaterial under solvent-free conditions has been effectively accomplished. The aromatic aldehydes, amines, and phenylacetylene were reacted at 100 degrees C in the presence of the resultant catalyst to form propargylamines. The nanocrystalline TiO2 was initially synthesized by a sol-gel method from titanium(iv) isopropoxide (TTIP) and further subjected to ZnCl2 loading by a wet impregnation method. X-ray diffraction (XRD) patterns revealed the formation of crystalline anatase phase TiO2. Field emission scanning electron microscopy (FESEM) showed the formation of agglomerated spheroid shaped particles having a size in the range of 25-45 nm. Transmission electron microscopy (TEM) validates cubical faceted and nanospheroid-like morphological features with clear faceted edges for the pure TiO2 sample. Surface loading of ZnCl2 on spheroid TiO2 nanoparticles is evident in the case of the ZnCl2 loaded TiO2 sample. X-ray photoelectron spectroscopy (XPS) confirmed the presence of Ti4+ and Zn2+ species in the ZnCl2 loaded TiO2 catalyst. Energy-dispersive X-ray (EDS) spectroscopy also confirmed the existence of Ti, O, Zn and Cl elements in the nanostructured catalyst. 15% ZnCl2 loaded TiO2 afforded the highest 97% yield for 3-(1-morpholino-3-phenylprop-2-ynyl)phenol, 2-(1-morpholino-3-phenylprop-2-ynyl)phenol and 4-(1,3-diphenylprop-2-ynyl)morpholine under solvent-free and aerobic conditions. The proposed nanostructure-based heterogeneous catalytic reaction protocol is sustainable, environment-friendly and offers economic viability in terms of recyclability of the catalyst.

引用

页码：32735 / 32743

页数：9

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