One-Pot Synthesis

The fabrication of supercapacitors with outstanding performance is presented with a distinct defect-rich nanostructures. A one-pot, energy-efficient method for synthesizing defective manganese dioxide nanowires doped with potassium (K 0.35 MnO2) was developed. The introduction of potassium ions at 35 % birnessite resulted in a significant increase in lattice defects and an improvement in conductivity. Addition of KOH induces a phase transition from α-MnO2 to δ-MnO2. These imperfections result in a greater quantity of active sites, which are crucial for the process of energy storage. The K 0.35 MnO2 structure demonstrates a 405F/g increased capacity at a current density of 1 A/g. The asymmetric supercapacitor (K 0.35 MnO2 /AC) that was manufactured exhibits a capacitance of 106.4F/g when operating at 1 A/g, while maintaining a maximum energy density of 71.5 Wh kg−1 and a power density of 672 W kg−1. Furthermore, 92.7 % of the initial capacitance of the device is retained even after 8,000 cycles at 20 A/g. This study presents novel insights into the production of defective materials for energy storage applications through the utilization of a one-pot process as opposed to the multi-step method. In order to produce high-performance supercapacitors for practical applications, the results indicate that defect engineering is a crucial factor.

Unless otherwise stated, all reactions were carried out under on oxygen free nitrogen atmosphere using predried solvents and standard Schlenk techniques, subsequent chromatographic and work up procedures were performed in air. All chemicals and Lawesson's reagent were purchased from Sigma-Aldrich without further purification. 2,4-diferrocenyl-1,3,2,4-diathiadiphosphetane 2,4-disulfide [FcP(μ-S)S]2 (FcLR), was prepared by using the literature method. s1,s2 1 H (400.1 MHz), 13 C (100.6 MHz) and 31 P-{ 1 H} (162.0 MHz) NMR spectra were recorded at 25 º C (unless stated otherwise) on Bruker Advance II 400. IR spectra were recorded as KBr pellets in the range of 4000-250 cm-1 on a Perkin-Elmer 2000 FTIR/Raman spectrometer. Mass spectrometry was performed by the EPSRC National Mass Spectrometry Service Centre, Swansea. X-ray diffraction data for compound 14 was collected at 125 K using the St Andrews Automated Robotic Diffractometer (STANDARD), s3 consisting of a sealed-tube generator (Rigaku, Houston, USA) equipped with a SHINE monochromator [Mo Kα radiation (λ = 0.71075 Å)], and a Saturn 724 CCD area detector, coupled with a Microglide goniometer head and an ACTOR SM robotic sample changer. Diffraction data for compounds 10a, 10b, 11, 12a and 12b were collected at either 93 K or 173 K (all other crystals) by using a Rigaku FR-X Ultrahigh Brilliance Microfocus RA generator/confocal optics and Rigaku XtaLAB P200 system, with Mo Kα radiation (λ = 0.71075 Å). Intensity data were collected using ω steps accumulating area detector images spanning at least a hemisphere of reciprocal space. All data were corrected for Lorentz polarization effects. A multi-scan absorption correction was applied by using CrystalClear. s4,s5 Structures were solved by either charge-flipping (SUPERFLIP) s6 or direct (SIR2004, SIR2011) s7,s8 methods, and refined by full-matrix leastsquares against F 2 (SHELXL-2013). s9 Non-hydrogen atoms were refined anisotropically, and hydrogen atoms were refined using a riding model. All calculations were performed using the CrystalStructure interface. s10 2. Synthesis and Characterization of Heterocycles 1-12 and 14

ChemInform Abstract The polyhydroxy benzenes (I) are acylated with phenylpropiolic acid (II) to yield the flavones (III) and (IV) by mixing the reagents with a thick polyphosphoric acid paste containing a few drops of concentrated sulfuric acid.

In order to treat the organic pollutants like dyes in water bodies, the environmentally benign nanoparticles are used extensively. The nanoparticles preparation by green chemistry approach is advantageous for this purpose. The Cu 2 O nanoparticles (NPs) were synthesized here by using Cu(NO 3) 2 and T. arjuna bark extract (as reducing and capping agent) under microwave irradiation. They were characterized by X-ray diffraction (XRD), Fourier transform infrared spectra (FT-IR), BET surface area and UV-vis spectra. The adsorption of methylene blue (MB) on Cu 2 O NPs in light and dark condition was found to be about 63% and 55%, respectively. The adsorption followed Langmuir isotherm, Freundlich isotherm and pseudo second order kinetics. The photo induced degradation of MB dye in presence of Cu 2 O NPs was also studied using photocatalytic reactor having UV lamp (250 W). Up to 97% degradation of MB occurred as monitored from UV-vis spectra. The degradation of MB was confirmed by HPLC and LC-MS analysis.

Bis(pyridin-1-ium)benzene trifluoroacetate coordinated to chloropropyl functionalized SiO 2-nano-NiFe 2 O 4 (BPBTCSF). Fourier-transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX), transmission electron microscopy (TEM), elemental mapping analysis, Brunauer-Emmett-Teller (BET), thermal gravimetric analysis (TGA), vibratingsample magnetometry (VSM) and X-ray diffraction (XRD) techniques characterized the framework of this catalyst. The catalytic activity of this nano-composite was then examined in the one-pot four-component reaction of 2-thiobarbituric acid, NH 4 OAc, and aldehyde for synthesis of pyrido[2,3-d:6,5-d']dipyrimidines under optimal conditions (5 mg of BPBTCSF, H 2 O, 25 • C). BPBTCSF exhibits benefits as a heterogeneous catalyst, such as exciting performance in the production of derivatives (2 to 5 min, 90 % to 98 %), six times reproducibility with a slight decrease in catalytic activity, the simultaneous presence of acidic and basic sites (Hydrogen attached to the electronegative nitrogen atom and CF 3 COOˉ, respectively), convenient purification and separation from the reaction mixture.

Organo-tin compounds S 4800 A Novel One-Pot Procedure for the Synthesis of Stable Dioxadiazastannepines and Dioxadiazasilepines.-Generation of the dianion from dioxime (I) and following reaction with dichlorostannanes or dichlorosilanes results in a short synthesis of the novel title heterocycles.-(SINGH*,

5-hydroxymethylfurfural (HMF) was selectively oxidized to 2,5-
furandicarboxylic acid (FDCA) using an effective catalytic system
made of Au particles supported on Ce-modified MgFe layered
double hydroxide. The structural features and performance of
the as-prepared catalysts were examined using a range of
characterizations, and the impact of altering reaction parameters
was explored. It was demonstrated that the presence and
quantity of Ce and Mg species in the catalyst formulation were
the primary determinants of the activity of the
Au@Mg􀀀 N􀀀 M􀀀 LDH catalysts (M=Ce, Cu, Mn, Zr, and N=Fe, Al).
The catalyst Au@MgFeCe􀀀 LDH, loaded with 1 wt% Au, exhibited
outstanding catalytic activity in the production of FDCA,
achieving complete HMF conversion and 90% FDCA selectivity.
This was accomplished through a two-step heating procedure,
involving initial heating of the reaction medium at 40°C for
2 hours followed by a subsequent heating at 100°C for 6 hours,
conducted under an oxygen pressure of 5 bar.

In this study, we present a simple, economical and environmentally friendly approach to synthesize 3,4-dihydropyrimidin-2(1H)-ones. This involves a one-pot, three-component condensation process using ethyl acetoacetate, an aldehyde, and urea. The reaction takes place efficiently with glacial acetic acid acting as a catalyst under grinding conditions, leading to good yields

A convenient and efficient route for synthesis of various derivatives of 3‐benzoyl‐4‐phenyl‐2‐(trifluoromethyl)pyrano[3,2‐c]chromen‐5(4H)‐one has been used via tandem Knoevenagel condensation–Michael addition and intramolecular cyclization sequence. These products have been synthesized in the presence of catalytic amount of metal–organic framework (MOF) and potassium carbonate as one‐pot, three‐component reaction. MOF catalyst has been separated easily with external magnet, and high purity of products has been obtained after washing with ethanol. This protocol has advantages of simplicity, mild condition, and high yield. More importantly, MOF has been easily recycled for three times.

In this investigation, firstly Y2O3: Tb +3 nano-powders with the approximate size of 80 nm was synthesized via sol-gel approach. Then, with the addition of Tetraethyl orthosilicate (TEOS) to the considered raw materials, the doped YSO compounds were produced in the presence of different amounts of SiO2 and crystallographic and microscopic structure and also the luminescence properties of the produced materials were evaluated. To study the formed phases and also particle size and morphology of Y2O3: Tb +3 and YSO: Tb +3 synthesized structures, X-ray diffraction (XRD) and field emission scanning electron microscope (FESEM) were used. In this research, interestingly it was seen that the addition of silica results in the severe grain growth and this size reaches to 300-400 nm. In addition, with the employment of photoluminescence analyzer, the optical properties of these materials were studied. Finally, it was determined that in a case that the quantity of consumed SiO2 phase is equal to the stoichiometric values required for the formation of Y2SiO5, the highest emission intensity is achieved and the higher amounts of SiO2 leads to the reduction of intensity.

In this work, one-pot synthesis of modified silica nanoparticles with long-chain alcohol 1-Octadecanol by stober method at 70 C is presented. Hydrophobicity of particles increased dramatically by increasing the amount of 1-Octadecanol up to 7 wt.%. Surface modification was completed during the first 90 minutes. Additional reaction time had no further effect. The most possible modification was obtained when the reaction took place at pH=8. Successful surface modification was confirmed by FT-IR spectroscopy, thermogravimetric analyses and contact angle measurements. X-ray diffraction patterns indicate an amorphous structure which did not significantly change by surface modification. Transmission electron microscopy images were used to investigate the morphology and dimension of the silica particles.

Reaction of 6-amino-2-methylthiouracil and 6-amino-1,3-dimethyluracil with equimoler amounts of cyclic ketones or cyclic 1,3-diketones and the appropriate aromatic aldehydes yielded regioselectivity a series of polycyclic pyrimido[4,5-b]quinoline and pyrido[2,3-d]pyrimidine derivatives in good yields.

Fe 3 O 4 nanoparticles were prepared hydrothermally and characterized by X-Ray diffraction spectroscopy (XRD), and scanning electron microscopy (SEM). It was found that these nanoparticles can act as an efficient catalyst in the degradation of Methylene blue dye in aqueous solution in a Fenton like system in presence of 30% perhydrol. Uv-Vis spectroscopy was used to determine the concentration of dye during optimization of different affecting factors such as pH, catalyst loading, and amount of the oxidant. Based on these results, 0.6 g/L of the catalyst and 0.32 mmol/L of the oxidant at pH=4.8 were selected as the optimum conditions and this resulted in a considerable degradation in less than 20 minutes. The catalyst was also found to be recyclable with no considerable decrease in its efficiency in successive runs.

A simple, efficient, and eco-friendly synthetic protocol has been developed for the synthesis of pyranoxanthenes via one pot three-component reaction. This reaction is between aromatic aldehyde, 2,2-dimethylchroman-7-ol and 1,3-cyclohexanedione by using molecular iodine in AcOH as a reaction medium under microwave irradiation. Utilizing this protocol a variety of xanthene derivatives were synthesized in excellent yields. The synthesized compounds were established based on the spectral data and single crystal X-ray diffraction analysis of 6f. The synthesized compounds were evaluated for their in vitro antimicrobial and antioxidant activity. The results clearly demonstrated that compounds 6j, 6m and 6n exhibited significant antibacterial activity against bacterial strains. The results of the molecular docking studies supported the antibacterial activity of the synthesized compounds.

A series of 2-amino-6,7-disubstituted-5-methyl-5,8-dihydropyrido[2,3-d]pyrimidin-4(3H)-one derivatives were synthesized through one-pot condensation of 2,6-diaminopyrimidin-4-one, aldehyde and acyclic 1,3-dicarbonyl compounds in glycol under microwave irradiation without catalyst. The protocol in the absence of catalyst has the advantage of good yield (89-95%), short reaction time and being environmentally friendly.

We report a simple and suitable method for the preparation of useful 2-trifluoromethylchromones in one step, in high yields and avoiding the use of solvents. We were able to detect the intermediate of this reaction. Furthermore a mechanism for the formation of the 7-methoxy-3-trifluoroacetyl-2-trifluoromethylchromone through the unexpected double trifluoroacetylation of 4-methoxy-2hydroxyacetophenone followed by dehydration is also proposed. All compounds are fully identified and characterized by spectroscopic techniques.

An efficient green route for the preparation of naphthoxazinones, applying a three-component one-pot condensation reaction of 2-naphthol, aromatic aldehyde and urea in the presence of nano silica supported ferric chloride under solvent-free conditions has been developed. The present procedure offers several advantages such as short reaction time, simple workup, recovery and reusability of the catalyst.

ZnO nanoparticles as a worthwhile and recyclable catalyst have been used for the one-pot synthesis of 1,8-dioxo-decahydroacridines and 1,8-dioxooctahydro-xanthenes via multi-component reactions under solvent-free conditions. The presented method is mild, environmentally friendly, inexpensive and highly effective to give the products in good to excellent yields.

An efficient green route for the preparation of naphthoxazinones, applying a three-component one-pot condensation reaction of 2-naphthol, aromatic aldehyde and urea in the presence of nano silica supported ferric chloride under solvent-free conditions has been developed. The present procedure offers several advantages such as short reaction time, simple workup, recovery and reusability of the catalyst.

ZnO nanoparticles as a worthwhile and recyclable catalyst have been used for the one-pot synthesis of 1,8-dioxo-decahydroacridines and 1,8-dioxooctahydro-xanthenes via multi-component reactions under solvent-free conditions. The presented method is mild, environmentally friendly, inexpensive and highly effective to give the products in good to excellent yields.

in Wiley Online Library (wileyonlinelibrary.com). 3-Arylaminomethylidenechroman-2-carboxamide has been synthesized by a one-pot three component reaction among 3-formylchromone, aromatic amine, and cyclohexyl isocyanide. 3-(N-alkylsubstitued/ unsubstituted)aminomethylidenechroman-2-carboxamides were synthesized by heating Passerini products derived from chromone-3-carbaldehyde with different aliphatic primary amines. The products obtained from the reactions of aliphatic primary amines readily form chromeno[2,3-c]pyrrole when heated in acetic acid. Bischromanones have also been synthesized using this methodology.

Abstract: Brønstedacidic ionic liquid 3-methyl-1-sulphonic acid imidazolium chloride {[Msim] Cl} is utilized as a highly efficient, inexpensive, mild and green catalyst for the synthesis of β-acetamido ketones by the one-pot multi-component coupling between acetophenones, ...

The preparation, characterization and catalytic application of a novel 1, 3, 5-Tris (2-hydroxyethyl) isocyanurate functionalized graphene oxide are described. The catalyst was characterized by nitrogen adsorption-desorption analysis, scanning electron microscopy (SEM) and Fourier transform infrared (FTIR) spectroscopy. The thermal stability of the material was also determined by thermal gravimetric analysis (TGA). The catalytic application of 1, 3, 5-Tris (2-hydroxyethyl) isocyanurate functionalized graphene oxide nanocatalyst was then investigated in the biginelli condensation of different aldehydes with urea and alkylacetoacetates under solvent-free conditions and at moderate temperature. Moreover, the significant advantages of this procedure are the stability, reactivity and reusability of the catalyst, low loading of the catalyst, avoiding the use of toxic transition metals, short reaction times, high to excellent yields, easy separation and purification of the products.

This article describes a simple protocol for the efficient synthesis of 3,4-dihydropyrimidin-2(1H)-one derivatives using aromatic aldehydes, ethyl acetoacetate and urea in the presence of nano-BBr3.SiO2 as a catalyst. The structural features of the synthesized compounds were characterized by m.p., IR, MS, H NMR, C NMR, and CHN elemental analysis. We synthesized nano-BBr3.SiO2 for the first time as a nanocatalyst and characterized it by XRD, SEM and TEM techniques. High yields, mild conditions, easy availability, reusability, and green chemistry were some advantages of using this catalyst.

In this study, the synthesis of 4 H -chromenes of biological activity via a multicomponent reaction of dimedone, aromatic aldehydes and malononitrile catalyzed by glutamic acid as a catalyst was investigated. The structural features of the synthesized compounds were characterized by melting point, IR and 1 H NMR analysis. The catalyst being reported here is cheap, safe to handle and the whole procedure is eco-friendly, Milder conditions, one-pot, excellent yields, operational simplicity and ecofriendly preparation are some advantages of this protocol. The compounds were screened for antimicrobial activity. The results showed that these compounds reacted against all the tested bacteria and fungi.

A wide variety of 2-amino-4H-chromene derivatives with diverse substituents on the 4H-chromene ring were efficiently prepared via one-pot, three-component reaction of an aromatic aldehyde, malononitrile (or ethyl cyanoacetate), and diverse enolizable C–H activated acidic compounds in the presence of low loading of potassium phthalimide-N-oxyl (POPINO), as a new organocatalyst, in aqueous media. This procedure is a clean, transition metal-free, and environmentally friendly approach to prepare different 2-amino-4H- ...

Synthetic application of Silica–ZnCl2 , as an efficient and eco‐friendly catalyst for the synthesis of a small library of dihydropyrimidinones is described in this report. The reaction involves a one pot, multicomponent reaction of β‐oxodithiocarboxylates, aldehydes, and urea under solvent‐free conditions. The experimental procedure is simple, environmental benign, tolerated with many functional groups, and results in good to excellent yield of the products.

Present work deals with the preparation of some Pyrazole derivative salts which was prepared by using different kinds of aldehydes and hydrazine derivatives by using alkoxide as a base and using the 1,3-dicarbonyl compound like ethyl acetoacetate at room temperature. The reaction mixture was stirred on magnetic stirrer for about 10 to 20 minutes till colour change is observed and then product is separated by using organic solvent. The product obtained was converted to sodium salt of Pyrazole derivative by base hydrolysis. The entire synthesized compound was tested for their antibacterial activity against the Gram-positive and Gram-negative strains of bacteria. The investigation of antibacterial screening data revealed that most of the tested compounds showed moderate to good antibacterial activity.

An efficient one-pot multi component synthesis of 1, 4-Polyhydroquinoline derivatives through unsymmetrical Hantzsch reaction using lanthanum chloride heptahydrate (LaCl3.7H2O) from an aromatic aldehyde, ethyl acetoacetate, dimedone and ammonium acetate as a nitrogen precursor in ethanol at room temperature is described. In the present work, we report lanthanum chloride heptahydrate remarkably non-toxic in nature and ease of handling, we explored the utility of lanthanum chloride heptahydrate as a catalyst for the synthesis of 1, 4polyhydroquinoline derivatives. We newly report p-N, N-dimethylaminocinnamaldehyde and m-chlorobenzaldehyde for the synthesis of 1, 4-Polyhydroquinoline derivatives through unsymmetrical Hantzsch reaction and the products were characterized by IR and 1 HNMR spectroscopic methods.

Cerpegin (1) was synthesized through a Ôone-potÕ reaction in 71% overall yield. Lithiation of commercially available 2methoxynicotinic acid (2) as its lithium salt using LTMP, followed by addition of acetone at low temperature and a specific acidic treatment of the intermediate 3 thus obtained, gave the 1,1-dimethyl-3,4-dioxo-1,3,4,5-tetrahydrofuro[3,4-c]pyridine (4). The latter was finally selectively alkylated using methyl iodide and caesium carbonate to afford cerpegin (1).

A simple procedure afforded novel spiroacenaphthylene derivatives in high yields at room temperature from acenaphthenequinone, malononitrile, and phenol derivatives using amino-functionalized silica (SBA-Pr-NH 2) as a heterogeneous efficient solid base catalyst. Using SBA-Pr-NH 2 in the current procedure presents several advantages, such as a simpler procedure, shorter reaction times, facile synthesis, and simpler work-up. Also, recycling of the catalyst was completed with no significant decrease in the activity of catalyst.

CO 2 Me NO 2 Me MeO EXPERIMENTAL SECTION General Remarks: Melting points were recorded on a Superfit (India) capillary melting point apparatus and are uncorrected. IR spectra were recorded on a JASCO-FT-IR model 5300 spectrometer using solid samples as KBr plates and liquid sample as thin film between NaCl plates. For all the compounds 1 H NMR (400 MHz) and 13 C NMR (100 MHz) spectra were recorded in deuterochloroform (CDCl 3) on a Bruker-AVANCE-400 spectrometer using tetramethylsilane (TMS, δ = 0) as an internal standard at room temperature. HRMS spectra were recorded on Bruker maXis ESI-TOF spectrometer. The X-ray diffraction measurements were carried out at 298 K on a Bruker SMART APEX CCD area detector system equipped with a graphite monochromator and a Mo-Kα fine-focus sealed tube (λ = 0.71073 Å). Methyl (E)-2-(3-methoxybenzylidene)-4-nitropentanoate (3a) This compound was prepared following the literature 1 procedure known for similar compound with some modification. To a stirred solution of methyl 3-acetoxy-3-(3-methoxyphenyl)-2-methylenepropanoate (1a) (3 mmol, 0.793 g) and nitroethane (2a) (9 mmol, 0.675 g) in DMF (12 mL) was added K 2 CO 3 (9 mmol, 1.25 g) and reaction mixture was stirred at room temperature for 4 hours. The reaction mixture was diluted with brine (12 mL), extracted with diethyl ether (3x15 mL). The combined organic layer was washed with water (10 mL) and dried over anhydrous Na 2 SO 4. Solvent was evaporated and the resulting crude product was purified by column chromatography (silica gel, 5% EtOAc in hexanes) to afford 3a in 90% (0.76 g) yield as a pale brown viscous liquid.

TiO 2 nanoparticles (TiO 2 NPs) worked as an efficient heterogeneous catalyst in a one-pot, three-component, and solvent free Mannich reaction; producing various b-aminocarbonyls in good yields, and with good stereoselectivities. The catalyst was easily separated from the reaction mixture and was recycled four times with no significant loss of its catalytic activity.

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Cyclopentanone is a promising building block in the conversion of biomass to fuels. It can be readily obtained from furanics derived from biomass and can be converted to intermediate products in the molecular weight range compatible with fuels via C-C bond forming reactions. Among them, aldol condensation is a promising route. Conventional MgO catalysts are intrinsically active to catalyze this reaction, but they usually exhibit low surface areas and low stability in the presence of liquid water. The nitrate-citrate combustion method results in high-surface-area oxides with high condensation activity, but they are still susceptible to water attack. Here, hydrophobic MgO-based catalysts functionalized with octadecyltrichlorosilane (OTS) are shown to exhibit remarkable stability in the liquid phase under conditions in which a conventional MgO deactivates in short time. A follow-up study investigates the effect of co-fed water on the MgO-catalyzed cyclopentanone self-aldol condensation...