ABSTRACT
In this research, mesoporous carbon (MC) with high efficiency (0.65 g yield from 1.0 g MCM-41 and 1.25 g sucrose) was successfully prepared by adding carbon precursor (sucrose) in a single step with ultrasonic waves, which reduces time and energy cost. Then, the Cu2+/Mesoporous carbon nanocatalyst (Cu2+/MC) was synthesized by adding Cu(NO3)2 in a single step and applied as a catalyst in amidation reactions of alcohols. Also, Cu2+/MC was characterized using different spectroscopic methods and techniques, including Fourier transform infrared spectroscopy (FT-IR), Field Emission Scanning Electron Microscopy (FE-SEM), N2 adsorption analysis (BET), X-ray diffraction analysis (XRD), Energy Dispersive X-ray (EDX), and Thermogravimetric Analysis (TGA). Moreover, to show the catalytic merits of Cu2+/MC, various primary and secondary amines and ammonium salts were applied in the amidation of alcohols. Easy synthesis method, recyclability, excellent yields (80-93%), and simple work-up are some noticeable strengths of using Cu2+/MC as a catalyst in this reaction.
Subject(s)
Alcohols , Carbon , Spectroscopy, Fourier Transform Infrared , Microscopy, Electron, ScanningABSTRACT
An effective method for synthesizing acridinedione derivatives using a xanthan gum (XG), Thiacalix[4]arene (TC4A), and iron oxide nanoparticles (IONP) have been employed to construct a stable composition, which is named Thiacalix[4]arene-Xanthan Gum@ Iron Oxide Nanoparticles (TC4A-XG@IONP). The process used to fabricate this nanocatalyst includes the in-situ magnetization of XG, its amine modification by APTES to get NH2-XG@IONP hydrogel, the synthesis of TC4A, its functionalization with epichlorohydrine, and eventually its covalent attachment onto the NH2-XG@IONP hydrogel. The structure of the TC4A-XG@IONP was characterized by different analytical methods including Fourier-transform infrared spectroscopy, X-Ray diffraction analysis (XRD), Energy Dispersive X-Ray, Thermal Gravimetry analysis, Brunauer-Emmett-Teller, Field Emission Scanning Electron Microscope and Vibration Sample Magnetomete. With magnetic saturation of 9.10 emu g-1 and ~ 73% char yields, the TC4As-XG@IONP catalytic system demonstrated superparamagnetic property and high thermal stability. The magnetic properties of the TC4A-XG@IONP nanocatalyst system imparted by IONP enable it to be conveniently isolated from the reaction mixture by using an external magnet. In the XRD pattern of the TC4As-XG@IONP nanocatalyst, characteristic peaks were observed. This nanocatalyst is used as an eco-friendly, heterogeneous, and green magnetic catalyst in the synthesis of acridinedione derivatives through the one-pot pseudo-four component reaction of dimedone, various aromatic aldehydes, and ammonium acetate or aniline/substituted aniline. A combination of 10 mg of catalyst (TC4A-XG@IONP), 2 mmol of dimedone, and 1 mmol of aldehyde at 80 °C in a ethanol at 25 mL round bottom flask, the greatest output of acridinedione was 92% in 20 min.This can be attributed to using TC4A-XG@IONP catalyst with several merits as follows: high porosity (pore volume 0.038 cm3 g-1 and Pore size 9.309 nm), large surface area (17.306 m2 g-1), three dimensional structures, and many catalytic sites to active the reactants. Additionally, the presented catalyst could be reused at least four times (92-71%) with little activity loss, suggesting its excellent stability in this multicomponent reaction. Nanocatalysts based on natural biopolymers in combination with magnetic nanoparticles and macrocycles may open up new horizons for researchers in the field.
ABSTRACT
In this work, graphitic carbon nitride-supported L-arginine (g-C3N4@L-arginine) nanocatalyst was synthesized and evaluated using FT-IR, EDX, XRD, TGA, and FESEM analyses. The performance of the prepared nanocatalyst was examined in the synthesis of 1,4-dihydropyridine, 4H-chromene, and 2,3-dihydro quinazoline derivatives. The novel g-C3N4@L-arginine nanocatalyst showed high thermal stability, easy separation from reaction media, the capability to be used in various multicomponent reactions, and acceptable reusability.