scholarly journals H3PW12O40 Anchored on the Three-Dimensional and Networked SBA-15 as an Efficient and Recyclable Catalyst for Mannich Reaction

Author(s):  
Tengfei Zhang ◽  
Wei Zhang ◽  
Hao Dong ◽  
Qing Liu

Abstract. The three-dimensional and networked SBA-15 (3D-SBA-15) supported phosphotungstic acid (PW) was used as heterogeneous catalyst for the one-pot three-components Mannich reaction at room temperature. The H3PW12O40/3D-SBA-15 catalyst was prepared using an impregnation method and confirmed by series of characterizations such as Fourier-transform infrared spectra (FT-IR), scanning electron microscope (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), N2 physisorption and thermogravimetric (TG) analysis. 50PW/3D-SBA-15 catalyst with H3PW12O40 loading of 50 wt% showed the highest yield of 93% in 1.8 h for the Mannich reaction of benzaldehyde, aniline and acetophenone under solvent-free condition. A series of β-aminoketone derivatives were synthesized successfully in the presence of this catalyst. In addition, H3PW12O40/3D-SBA-15 catalyst can be easily recovered and reused four times without significant decrease of the activity. This work provides an improved modification of the three-component Mannich reaction in terms of mild reaction conditions, clean reaction profiles, small quantity of catalyst and a simple workup procedure.                                                Resumen.  El ácido fosfotungstico (PW) se soportó en sílice SBA-15 (3D-SBA-15) y se usó como catalizador heterogéneo en la reacción de Mannich en un solo paso de tres componentes a temperatura ambiente. El catalizador H3PW12O40/3D-SBA-15 se preparó mediante impregnación y se caracterizó por espectroscopia de infrarrojo (FT-IR), microscopia electrónica de barrido (SEM), microscopía electrónica de transmisión (TEM), difracción de rayos-X (XRD), fisisorción de N2 y análisis termogravimétrico (TG). El catalizador 50PW/3D-SBA-15, con una carga de H3PW12O40 del 50% en peso, mostró el rendimiento más alto del 93% en 1.8 h para la reacción de Mannich entre benzaldehído, anilina y acetofenona, sin disolvente. Se sintetizó una serie de derivados de β-aminocetona en presencia de este catalizador. Además, el catalizador H3PW12O40/3D-SBA-15 puede recuperarse fácilmente y reutilizarse cuatro veces sin pérdida significativa de la actividad. Este trabajo reporta una modificación de la reacción de Mannich de tres componentes bajo condiciones de reacción suaves, perfiles de reacción limpios, pequeña cantidad de catalizador y un procedimiento de tratamiento simple.

NANO ◽  
2018 ◽  
Vol 13 (06) ◽  
pp. 1850063 ◽  
Author(s):  
Jinhua Zhang ◽  
Huiyue Qian ◽  
Wencheng Liu ◽  
Hao Chen ◽  
Yang Qu ◽  
...  

A heterostructural composite composed of g-C3N4 and Bi2O3 was achieved by the one-pot and thermal-induced polycondensation method using melamine and Bi(NO[Formula: see text] as precursor at 550[Formula: see text]C under air atmosphere. The crystalline phase, components and morphologies of the as-prepared composites were investigated by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM). Besides, the photocatalytic activity of composites was evaluated by degrading RhB aqueous solution at room temperature under visible light irradiation. Compared with bulk g-C3N4, the photocatalytic efficiency of the 0.5% Bi2O3/g-C3N4 (Bi–CN) was increased by up to four times. The introduction of Bi2O3 enhances not only the light absorption ability, but also the separation of photogenerated electron–hole pairs.


2021 ◽  
Author(s):  
Fatemeh Samandi Zadeh ◽  
Mohammad Kazem Mohammadi ◽  
Ayeh Raeiatzadeh ◽  
Neda Hasanzadeh

Abstract The simple and efficient synthesis reaction was used for preparing Bis (dihydropyrimidinone) derivatives through Biginelli condensation reaction of terephthalic aldehyde, 1, 3-dicarbonyl compounds and (thio) urea or guanidine and tetrahydro-4H-chromenes via one pot condensation of aromatic aldehydes, malononitrile and dimedone with Ag2O/GO/TiO2 composite nanostructures as a catalyst. The structural functionalities and morphological observations of catalyst were obtained using characterization techniques of field emission scanning electron microscopy (FESEM), X-ray diffraction (XRD), Fourier transfer infrared (FT-IR) spectroscopy and transmission electron microscope (TEM). The structures of Bis (dihydropyrimidinone) and tetrahydro-4H-chromenes confirmed by FT- IR, NMR and mass spectroscopy. Excellent yields of the products, simple reaction process and simple work-up are attractive features of these effective synthesis methods.


2020 ◽  
Vol 26 (1) ◽  
pp. 26-32 ◽  
Author(s):  
Nader Noroozi Pesyan ◽  
Narmin Akhteh ◽  
Hana Batmani ◽  
Barış Anıl ◽  
Ertan Şahin

AbstractAn easy and convenient technique for the one-pot synthesis of novel compounds of hexahydroacridine-1,8(2H,5H)-dione and octahydroacridin-10(1H)-yl) thiourea derivatives has been developed by the reaction of the octahydro-1H-xanthenes with hydroxylamine hydrochloride and thiosemicarbazide in ethylene glycol, which is a green solvent, under mild reaction conditions. IR, 1H NMR, 13C NMR spectrometry, and X-ray diffraction analysis were used to identify the structures of these compounds.


2012 ◽  
Vol 455-456 ◽  
pp. 1053-1059
Author(s):  
Xue Hai Fan ◽  
Guo Min Xiao

Multi-walled carbon nanotubes (MWCNTs), potassium dichromate (K2Cr2O7) and sulphuric acid were used for the preparation of Cr/MWCNT composite by impregnation method. The composites were comprehensively characterized by transmission electron microscopy (TEM),energy dispersive X-ray analysis (EDX), infrared spectroscopy (FT-IR), X-ray diffraction (XRD) and thermal gravity analysis (TGA). Due to its unique electrical and structural properties, this composite was applied to the synthesis of biodiesel (FAME) as a catalyst, showing effectively catalytic performance.


2018 ◽  
Vol 2018 ◽  
pp. 1-10 ◽  
Author(s):  
Hui-qiang Wang ◽  
Ming-hua Liu ◽  
Xin Luo ◽  
Yi-fan Liu ◽  
Fei-er Chen ◽  
...  

ZnFe2O4/AC composites were prepared by the one-pot hydrothermal method using the activated carbon (AC) as a carrier. The synthesis conditions were optimized by a single-factor experiment. The structural, textural, and surface properties of the adsorbent have been comprehensively characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier-transform infrared (FT-IR) spectroscopy, Brunauer–Emmett–Teller (BET) measurements, and X-ray photoelectron spectroscopy (XPS) analysis. The SO2 removal capacities of the composites were investigated via testing the adsorption capacity at the self-made desulfurization equipment. The results show that the adsorption capacity of ZnFe2O4/AC composites is much higher than that of the AC and ZnFe2O4 samples, respectively. The composite overcomes the disadvantages of the traditional sintering, showing a very high desulfurization performance. The breakthrough time was 147 min, and the sulfur adsorption capacity could reach 23.67% in the desulfurization performance test.


2020 ◽  
Author(s):  
Fatemeh Samandi Zadeh ◽  
Mohammad Kazem Mohammadi ◽  
Ayeh Rayatzadeh ◽  
Neda Hasanzadeh

Abstract The simple and efficient synthesis reaction was used for preparing Bis (dihydropyrimidinone) derivatives through Biginelli condensation reaction of terephthalic aldehyde, 1, 3-dicarbonyl compounds and (thio) urea or guanidine and tetrahydro-4H-chromenes via one pot condensation of aromatic aldehydes, malononitrile and dimedone with Ag2O/GO/TiO2 composite nanostructures as a catalyst. The structural functionalities and morphological observations of catalyst were obtained using characterization techniques of field emission scanning electron microscopy (FESEM), X-ray diffraction (XRD), Fourier transfer infrared (FT-IR) spectroscopy and transmission electron microscope (TEM). The structures of Bis (dihydropyrimidinone) and tetrahydro-4H-chromenes confirmed by FT- IR, NMR and mass spectroscopy. Excellent yields of the products, simple reaction process and simple work-up are attractive features of these effective synthesis methods.


2014 ◽  
Vol 70 (11) ◽  
pp. 1069-1074 ◽  
Author(s):  
Jeffrey A. Rood ◽  
Steven Boyer ◽  
Allen G. Oliver

Reaction of cadmium nitrate with diphenylphosphinic acid in dimethylformamide solvent yielded the one-dimensional coordination polymercatena-poly[[bis(dimethylformamide-κO)cadmium(II)]-bis(μ-diphenylphosphinato-κ2O:O′)], [Cd(C12H10O2P)2(C3H7NO)2]n, (I). Addition of 4,4′-bipyridine to the synthesis afforded a two-dimensional extended structure, poly[[(μ-4,4′-bipyridine-κ2N:N′)bis(μ-diphenylphosphinato-κ2O:O′)cadmium(II)] dimethylformamide monosolvate], {[Cd(C12H10O2P)2(C10H8N2)]·C3H7NO}n, (II). In (II), the 4,4′-bipyridine molecules link the CdIIcenters in the crystallographicadirection, while the phosphinate ligands link the CdIIcenters in the crystallographicbdirection to complete a two-dimensional sheet structure. Consideration of additional π–π interactions of the phenyl rings in (II) produces a three-dimensional structure with channels that encapsulate dimethylformamide molecules as solvent of crystallization. Both compounds were characterized by single-crystal X-ray diffraction and FT–IR analysis.


NANO ◽  
2014 ◽  
Vol 09 (07) ◽  
pp. 1450084 ◽  
Author(s):  
HAIQIU LIU ◽  
YUJIAN JIN ◽  
NA LI ◽  
LILI WANG ◽  
SUNQI LOU ◽  
...  

Three-dimensional (3D) γ- MnOOH networks are successfully prepared by one-pot solvothermal method without using any catalyst. The samples are characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and high-resolution transmission electron microscopy (HRTEM). It is found that the amounts of urea and H 2 O 2 added, reaction temperature and time have important influences on the samples. It is interesting that the 3D networks are formed from the oriented attachment (OA) of Mn 3 O 4 octahedrons; and that the phase transformation from Mn 3 O 4 to γ- MnOOH occurs via the protonation of Mn 3 O 4. This study is expected to offer a facile approach to the syntheses of new, intricate nanostructures.


Scientifica ◽  
2016 ◽  
Vol 2016 ◽  
pp. 1-13 ◽  
Author(s):  
Vidhisha Jassal ◽  
Uma Shanker ◽  
B. S. Kaith

Prussian blue analogue potassium metal hexacyanoferrate (KMHCF) nanoparticles Fe4[Fe(CN)6]3(FeHCF), K2Cu3[Fe(CN)6]2(KCuHCF), K2Ni[Fe(CN)6]·3H2O (KNiHCF), and K2Co[Fe(CN)6] (KCoHCF) have been synthesized using plant based biosurfactantAegle marmelos(Bael) and water as a green solvent. It must be emphasized here that no harmful reagent or solvent was used throughout the study. Plant extracts are easily biodegradable and therefore do not cause any harm to the environment. Hence, the proposed method of synthesis of various KMHCF nanoparticles followed a green path. The synthesized nanoparticles were characterized by powder X-ray diffraction (PXRD), Field-Emission Scanning Electron Microscopy (FE-SEM), Transmission Electron Microscopy (TEM), and Fourier Transform Infrared Spectroscopy (FT-IR). MHCF nanoparticles were used for the photocatalytic degradation of toxic dyes like Malachite Green (MG), Eriochrome Black T (EBT), Methyl Orange (MO), and Methylene Blue (MB). Under optimized reaction conditions, maximum photocatalytic degradation was achieved in case of KCuHCF nanoparticles mediated degradation process (MG: 96.06%, EBT: 83.03%, MB: 94.72%, and MO: 63.71%) followed by KNiHCF (MG: 95%, EBT: 80.32%, MB: 91.35%, and MO: 59.42%), KCoHCF (MG: 91.45%, EBT: 78.84%, MB: 89.28%, and MO: 58.20%).


2014 ◽  
Vol 989-994 ◽  
pp. 134-137
Author(s):  
Yuan Yuan She ◽  
Xuan Yan Liu ◽  
Zhi Gao Yang

Sucrose char sulfonic acid (SCSA) efficiently catalyzed the one-pot, three-component Mannich reaction of ketones, aromatic aldehydes and different amines in ethanol at 30°C and afforded the corresponding β-amino carbonyl compounds in good to excellent yields . This method provides a novel and improved modification of the three-component Mannich reaction in terms of mild reaction conditions , clean reaction profiles and a simple workup procedure.


Sign in / Sign up

Export Citation Format

Share Document