A PCl3-mediated conversion of tert-butyl esters into esters and amides in one-pot under air is developed. This novel protocol is highlighted by the synthesis of skeletons of bioactive molecules and gram-scale reactions. Mechanistic studies revealed that this transformation involves the formation of an acid chloride in situ, which is followed by reactions with alcohols or amines to afford the desired

The effect of carbon nanotubes on the catalytic properties of Rh-Mn-Li/SiO2 catalysts was investigated for CO hydrogenation. The catalysts were comprehensively characterized by means of X-ray power diffraction, N2 sorption, transmission electron microscope, H2–temperature-programmed reduction, CO–temperature-programmed desorption, temperature-programmed surface reaction, and X-ray photoelectron spectroscopy

A coordination compound constructed from a nitronyl nitroxide biradical NITPh(3-NIT) and CuII(hfac)2(H2O)2 building blocks [NITPh(3-NIT) = 1,3-bis(1′-oxyl-3′-oxido-4′,4′, 5′, 5′-tetramethyl-4,5-dihydro-1H-imidazol-2-y1)-benzene, hfac = hexafluoroacetylacetonato] is successfully synthesized. The crystal structure is determined by X-ray single-crystal diffraction. The asymmetric complex {[(NITPh(3-NIT)]Cu(hfac)2}

The mechanisms of several types of thiol-independent peptide ligation reported over the past 14 years have been reviewed.

Eleven glycosyl coumarylthiazole derivatives are synthesized by cyclization and condensation of glycosyl thiourea with 3-bromoacetyl coumarins in ethanol. The reaction conditions are optimized and good yields of products (80%–95%) are obtained. The structures of all new products were confirmed by IR, 1H and 13C NMR, and by HRMS (electrospray ionization). The in vitro acetylcholinesterase (AChE) inhibitory

A new taraxerane-type triterpenoid, codopimodol A (1), together with two known triterpenoids (2 and 3), were isolated from the EtOH extract of the roots of Codonopsis pilosula var. modesta (Campanulaceae). The structure of the new compound was identified by high-resolution electrospray ionization mass spectrometry and extensive spectroscopic analyses, particularly one-dimensional and two-dimensional

Aflatoxins are extremely harmful carcinogens to humans and animals. In recent years, attention has been directed toward the application of molecular imprinting polymers for the separation and detection of aflatoxin. In this review, polymerization methods for the preparation of molecular imprinting polymers for aflatoxin detection, such as lump-bulk polymerization, spherical molecular imprinting polymer

A new silver(I) complex of the type [Ag2(mbbp)2](pic)2·DMF·CH3OH [mbbp = 2,6-bis(N-methylbenzimidazol-2-yl)pyridine] is synthesized and analyzed using a range of spectroscopic and crystallographic techniques. This compound contains cationic Ag2(mbbp)2 dimers, in which the crossed eight-shaped structure is formed by two mbbp ligands bridging two silver(I) centers and Ag–Ag bonds. Two-dimensional supramolecular

Comparative molecular docking studies on creatine and guanidinoacetic acid, as well as their phosphorylated analogues, creatine phosphate, and phosphorylated guanidinoacetic acid, are investigated. Docking and density functional theory studies are carried out for muscle creatine kinase. The changes in the geometries of the ligands before and after binding to the enzyme are investigated to explain the

Four 2-phenylthiazole derivatives are synthesized, characterized, and evaluated as cholinesterase inhibitors. The structures of the 2-phenylthiazole derivatives are confirmed by 1H and 13C nuclear magnetic resonance spectroscopy, single-crystal X-ray diffraction studies, and Hirshfeld surfaces analysis. Hirshfeld surface analysis of the prepared compounds showed C–H···O intermolecular interactions

The dye mixtures formed from three commercial hair colour formers were purified by absorption onto human hair wefts, washed and dried, extracted with dichloromethane:trifluoroacetic acid (75:25) and then analysed by liquid chromatography–mass spectrometry. Only 1–2 dyes were identified from each complex mixture of commercial aromatic amines along with a broad UV absorption mainly consisting of mixtures

Activated carbons are prepared from coffee husks by chemical activation with ZnCl2 and are characterized by employing Brunauer, Emmett and Teller, scanning electron microscopy, Fourier-transform infrared spectroscopy, and Boehm titrations. The effects of ZnCl2/coffee husks, activation temperature, and activation time are studied, and the results show that the sample ACZ3-600-2 has a high surface area

Fifty-five 8-hydroxyquinoline (8-HQ) derivatives are synthesized and the corresponding aluminum(III), cadmium(II), copper(II), and zinc(II) metal complexes are prepared and their fluorescent activities are evaluated. The results indicate that the aluminum complexes have the best fluorescence properties, followed by zinc and cadmium complexes, while almost no fluorescence is observed with the copper

An efficient approach for the synthesis of pyrazoline/pyrazole-tethered pyridinyl methanones is described via a one-pot, stepwise, sequential methodology using chalcones and pyridine-4-carbohydrazide as substrates through a Michael addition followed by cyclization. The reaction proceeds via a catalyst-, solvent-, work-up-, and column-chromatography-free method under melt conditions to provide the pyrazolines

An array of 3-alkyl-1,2,3-triazol-1-ium hydrogen sulphate derivatives was obtained from the reaction between some 1,4-disubstituted-1,2,3-triazoles and H2SO4 through a simple protocol in good yields. The molecular structure of a triazolium salt (R1 = PhCH2, R2 = CH2O(4-CHO)C6H4) was unambiguously determined from X-ray diffraction studies, showing a remarkable triazole N3–H bond.

A highly selective OFF–ON fluorescent probe is developed for the sensing of Cu2+ based on the hydrolysis of a quinoline-2-carboxylate moiety. The probe is weakly fluorescent due to esterification of the phenolic group. Upon treatment with 1 equiv. of Cu2+, the probe exhibits strong fluorescence at 570 nm. The probe also exhibits high selectivity for Cu2+ over other cations with a low detection limit

Hydroxy-α-sanshool was synthesized in a 13% overall yield through eight steps, which included two Wittig reactions that were used to form the carbon skeleton with ethyl 2-oxoacetate and 2E,4E-hexadienal being reacted with the appropriate ylides. Impurities in the processes could easily be separated. Ethyl 6-hydroxy-2Z-hexenoate was converted to its E-isomer with catalysis by I2 and 2E,6Z,8E,10E-dodecatetraenoic

The acidic hydrolysis of astilbin to produce its aglycone, taxifolin, was investigated in this study. The effects of aq. HCl concentration and temperature on the reaction were studied, and the kinetic parameters were calculated. The results showed that with higher aq. HCl concentration and temperature, the hydrolysis of astilbin became faster. The activation energy of the hydrolysis reaction under

One organic compound [HMCA]2 (1) and two novel cobalt complexes [Co(MCA)(bipy)(H2O)]·(H2O) (2), [Co2(MCA)2(Phen)3]·3(H2O) (3) are synthesized by a solvothermal approach and are structurally determined by single-crystal X-ray diffraction. Compound 1 exhibits a two-dimensional structure by hydrogen bond and π. . .π stacking interaction. The complexes exhibit a three-dimensional and one-dimensional metal-organic

A series of extra-large micropore Sn-zeolites with different Si/Sn ratios is post-synthesized by treating the interlayer-expanded material ECNU-9-cal773 with a solution of HCl containing NH4F and SnCl4∙5H2O, named as IEZ-Sn-PLS-3(S4R). During treatment, HCl, NH4F, and SnCl4∙5H2O are hydrolyzed into H+, F+, and Sn4+ ions. The formation of a small amount of HF formed from H+ and F+ ions can corrode the

The absorption and desorption data of CO2 in aqueous solutions with a mass fraction of 10% and 20% of diethylenetriamine are measured at 313.15, 343.15, 373.15, and 393.15 K. The electrolyte non-random two-liquid theory is developed using Aspen V9.0 to correlate and predict the vapor–liquid equilibrium of CO2 in aqueous diethylenetriamine solutions. The model predicted the heat capacity and saturated

An efficient and high-yielding synthetic method for the preparation of vildagliptin via four steps is reported. The process starts from L-proline and involves a successful reaction with chloroacetyl chloride in tetrahydrofuran to afford (S)-1-(2-chloroacetyl)pyrrolidine-2-carboxylic acid, followed by a reaction with acetonitrile in the presence of sulfuric acid to give (S)-1-(2-chloroacetyl)pyrrol

Ir and Rh “PNP” complexes with different ligands are utilized for the oxidation of n-octane. Based on the obtained conversion, selectivity, and the characterized recovered catalysts, it is found that the combination of Ir and the studied ligands does not promote the redox mechanism that is known to result in selective formation of oxo and peroxo compounds [desired species for C(1) activation]. Instead

The aim of this study is to develop self-standing, ultrathin film, nanosheets with high magnetic response for use in a medical device that can be migrated to a target location in the body by using an external magnetic field. First, iron oxide nanoparticles are synthesized by either the sol-gel method or thermal decomposition. The resulting magnetic properties of the nanoparticles show that the thermal

Catalysts based on inexpensive and abundant transition metals are necessary for effective environmental remediation. In this study, a series of CuMn-CeO2 catalysts is synthesized by a simple coprecipitation method. The properties of the as-prepared catalysts are characterized by X-ray diffraction, Brunauer–Emmett–Teller analysis, scanning electron microscopy–energy-dispersive spectroscopy, transmission

Bendamustine deschloro dimer was considered as a potential impurity in bendamustine hydrochloride resulting from the hydrolysis of bendamustine followed by intermolecular esterification. An efficient synthesis of bendamustine deschloro dimer was achieved from 4-(5-amino-1-methyl-1H-benzo[d]imidazol-2-yl)butanoate involving nine sequential steps including benzyl-protection/deprotection of the amine

In this study, the mechanism for both the Huisgen 1,3-dipolar cycloaddition and the base-catalyzed cycloaddition reactions between phenylacetylene and azidobenzene has been investigated with density functional theory, namely at the M06-2X/6-31G(d) computational level. Later, the reaction has been modeled with a representative simple alkyne and a simple azide to concentrate solely on how the difference

An efficient, one-pot synthesis of 3-substituted-4H-[1,2,3]triazolo[5,1-c][1,4]oxazin-6(7H)-ones is developed via sequential esterification, substitution, and 1,3-dipolar cycloaddition processes of various propargyl alcohols, chloroacetyl chloride, and sodium azide. This method provides a variety of novel 1,2,3-triazole-fused oxazinones and has several advantages including simple operation, high efficiency

Two novel RE–Hg (RE = rare earth) complexes [RE(IA)3(H3O)2]2n·2n(HgCl4)·n(HgCl5)·nH2O·3nH3O (RE = Y, 1; Lu, 2; IA = isonicotinic acid anion) were synthesized through hydrothermal reactions and are structurally characterized by single-crystal X-ray diffraction. The two complexes are isostructures and are characteristic of a one-dimensional chain-like structure. Both complexes are characterized by a

1,3-Bis-(2-methyl-2-propenyl)benzimidazolium chloride and its Ag(I) complex are synthesized and the structures are elucidated using spectroscopies techniques. The molecular and crystal structures of the benzimidazolium salt are confirmed by X-ray crystallography. The molecular geometries of the benzimidazolium and its Ag(I) salt are analyzed using the B3LYP functional with the 6–311+G(d,p)/LANL2DZ

An efficient copper-catalyzed strategy for the synthesis of α-ketoamides via cross-coupling of methyl ketones and pyridin-2-amines is described. This transformation has provided a simple process for the formation of C−N and C=O bonds to prepare α-ketoamides, which are important substrates and intermediates for the preparation of fine chemicals. The reaction mechanism is investigated, which suggests

A novel chloro- and BF2bdk-substituted dithienylethene derivative, in which a chlorine atom and a difluoroboron β-diketonate (BF2bdk) group are appended at the termini of the dithienylethene core, is developed. The structure was confirmed by 1H NMR, 13C NMR, and high-resolution mass spectrometry (electrospray ionization). It displayed solvent-dependent photophysical properties, and blue/red light-triggered

Ethyl 2-(2-(1H-indol-3-yl)benzo[d]thiazol-3(2H)-yl)-2-cyanoacetate or acetate 6a–f as a series of novel compounds were synthesized from the reactions of benzothiazole, 2-methylbenzothiazole, or 2,5-dimethylbenzothiazole and ethyl bromocyanoacetate with indole derivatives. The reactions proceeded in acetone as a solvent under reflux for 5 h in good yields. The structures of new compounds were confirmed

Photoelectrochemical biofuel cells can convert light and chemical energy into electrical energy using a dye-sensitized titania (TiO2) fluorine-doped tin oxide photoanode and a platinum-coated fluorine-doped tin oxide cathode. TiO2 of the photoanode serves both as a support for dyes and as an electron-transporting medium, the structure of which can limit electron trapping and charge transporting and

Blue fluorescent carbon dots are synthesized via a one-step hydrothermal method using rosemary leaves as a carbon source. The obtained carbon dots are characterized by X-ray diffraction, transmission electron microscopy, X-ray photoelectron spectroscopy, UV-Vis, FTIR, and fluorescence spectrometry. The results show that carbon dots gave a maximum emission peak at 422 nm when excited at 332 nm. The

An efficient one-pot base-mediated approach to (E)-2-aroyl-4-arylidene-5-oxotetrahydro-furans is developed. Nine (E)-2-aroyl-4-arylidene-5-oxotetrahydrofurans are synthesized in good yields via tandem Passerini and cyclization reactions, starting from Baylis–Hillman acids, aryl glyoxals, and isocyanides at room temperature in the presence of Cs2CO3. In addition, the MTT assay is used to evaluate their

An efficient synthetic approach for the preparation of densely substituted furans starting from (E)-ethyl 3-aryl-2-cyanoacrylates and ethyl glycinate hydrochloride mediated by 1,8-diazabicyclo[5.4.0]undec-7-ene in the presence of water is investigated. The reactions are carried out under mild conditions in N,N-dimethylformamide at 95 °C. The products are cleanly obtained in 50%–57% yields, resulting

A synthesis of benzo[e][1,2,4]triazines and 1,2,4-triazolospiro[4,5]deca-2,6,9-trien-8-ones has been developed from reactions of amidrazones with 2-chloro-1,4-benzoquinone in EtOAc containing 0.5 mL of piperidine. This highly regioselective and one-pot process provided rapid access to 1,2,4-triazolospiro[4,5]deca-2,6,9-trien-8-ones (60%–70%) and benzo[e][1,2,4]triazines (11%–18%). On reacting amidrazones

The kinetics of the formation of the light orange–coloured complex [Ru(CN)5D-PA]3− are studied spectrophotometrically through substitution of a coordinated H2O molecule in aquapentacyanoruthenate(II) [Ru(CN)5OH2]3− by interaction with D-penicillamine [D-PA] in aqueous medium at 490 nm (λmax of [Ru(CN)5D-PA]3−). The reaction is monitored under pseudo-first-order conditions, taking [D-PA] in excess over

KRN7000 is particularly useful because it is a powerful and specific CD1d agonist and has prompted intense interest in the context of immunology in the past 25 years. Its limited commercial availability and high price has led to the publication of many different syntheses. However, almost all of them focused on the methodology development rather than a scalable synthesis. Herein, we have described

The synthesis and X-ray structure of a novel glycoluril derivative are described. The crystal of the glycoluril derivative is obtained by slow evaporation in a refrigerator at about 5 °C. X-ray crystallographic analysis revealed that the compound crystallized in an unusual as conformation instead of the usual clip-shaped aa conformation. Structural analysis shows that the solvation effect, hydrogen

Chamaejasmone F, a new 11,10-guaiane-type sesquiterpenoid, is isolated from the roots of Stellera chamaejasme Linn., along with four known compounds including two guaiane sesquiterpenoids and two lignans. The structure of the new compound is elucidated by extensive spectroscopic analysis, especially two-dimensional nuclear magnetic resonance spectroscopy and high-resolution electrospray ionization

In this paper, we report the synthesis of novel 1H-pyrano[2,3-d]pyrimidine-2,4(3H,5H)-dione derivatives 5(a–j) by a facile multicomponent reaction. The structures of all the newly synthesized compounds were characterized by different spectroscopic techniques including infrared, nuclear magnetic resonance (1H and 13C) and mass spectral analysis. All the new compounds were assessed for their in vitro

A one-pot method for the synthesis of azo compounds by the reaction of β-naphthol with aryl amines using t-BuONO as the nitrosonium source in DCM at room temperature was developed. This method features mild reaction conditions, a simple experimental procedure, and is free of acidic or alkaline additives.

Mixed ligand complexes of cobalt and palladium containing triphenylphosphine and a hydrazone derived from furfural and hydrazine hydrate have been designed, synthesized, evaluated, and characterized from their spectral properties, elemental analysis, and magnetic susceptibility measurements. The spectral techniques suggest that the complexes exhibit square planar geometry. The monomeric properties

Ni(NH3)4(AFT)2 [NiC6H16N18O2, AFT = 4-amino-3-(5-tetrazolate)furazan] is synthesized and characterized by elemental analysis and Fourier-transform infrared spectroscopy for the first time. X-ray diffraction measurements are used to determine the crystal structure of compound 1. The results demonstrate that compound 1 crystallized in the orthorhombic crystal system. The nickel(II) ion is six-coordinated

The ground and lowest singlet excited state geometries of selected (para-C5H4X)Ir(PH3)3 iridabenzene complexes (para-substituent = NH2, OMe, Me, H, F, Cl, CCl3, CF3, NO2) are optimized using the MPW1PW91 procedure employing the LanL2DZ(Ir) and 6-311G(d, p) (C, H, N, O, P, F, Cl, P) basis sets. The excited state is generated using the time-dependent density function method. The effects of electron-donating

Ferrocenyl imidazolo[2,1-b]-1,3,4-thiadiazoles are synthesized using 2-amino-5-substituted-1,3,4-thiadiazole and α-bromoacetyl ferrocene as substrates under microwave-assisted and catalyst-free conditions. The structures are characterized by infrared, 1H nuclear magnetic resonance, 13C nuclear magnetic resonance, mass spectrometry, and elemental analysis. Compared with conventional methods, the present

2,2’-Bipyridine with strong coordination ability for metal ions was used to prepare N-doped porous carbon materials by a facile method of solution agitation and annealing, with KOH as the activated solvent. Applied to supercapacitors, these porous carbon materials exhibit high specific capacitance and outstanding rate performance, which are attributed to their larger specific surface area, richer pore

The support used in a composite catalyst has an important influence on the catalytic performance of the catalyst. Amorphous metals have good electron-transfer properties and the presence of defect structures on the surface will introduce additional active sites and should be excellent catalyst supports. In this study, an [email protected] composite catalyst with amorphous Cu (a-Cu) as the support is

Organosulfur compounds with unsymmetrical S–S bonds are usually called unsymmetrical disulfides and are widely used in the biological, medicinal, and chemical fields. Their versatility has guided the development of various new methods for the synthesis of disulfides. In recent years, the synthesis of disulfides by cross-dehydrogenation of thiols has attracted much attention due to its high atomic economy

Carbon-based materials with multidimensional structures generally exhibit improved properties compared with single-morphology carbon materials for various applications including catalysis, adsorption, and energy storage. Here, an N-doped mesoporous carbon sphere and sheet composite is prepared by a co-assembly strategy using an ionic liquid ([C18Mim]Br) as the structure-directing agent, ethylenediamine

In this study, we report an investigation into the steric (cone angle, θ) and electronic properties of ligands in Ru-catalyzed C–H arylation of aromatic benzamides bearing 8-aminoquinoline as an N,N’-bidentate-directing group. The study employs [RuCl2(p-cymene)]2 as a precatalyst, and a ligand, under study, as a cocatalyst. Various electronically and sterically different monodentate and bidentate phosphine

The synthesis of C-ring quinoxaline-substituted sinomenine 1,2,3-triazole derivatives at the 4-OH via click reactions is accomplished, and a total of 16 novel sinomenine double N-heterocyclic derivatives are obtained in 74%–95% yields. The C-ring is first transformed into a 1,2-diketone structure under the action of hydrochloric acid, and then reacted with o-phenylenediamine to obtain a C-ring qui

In this work, tungsten oxide thin films are deposited on silicon substrates using the hot filament chemical vapor deposition system. The influence of substrate temperature on the structural, morphological, and elemental composition of the tungsten oxide thin films is investigated using X-ray diffraction, field-emission scanning electron microscopy, and X-ray photoelectron spectroscopy techniques. Also

A Re(I) complex of 3,3′-diamino-2,2′-bipyridine reacts irreversibly with aldehydes and unhindered ketones in water to form bis-aminal cyclised derivatives with the solid-state structure of the reaction with benzaldehyde reported. This reaction produces a Re(I) complex which is significantly more emissive than the starting compound.

A new cadinane-type sesquiterpene named cornifronone is isolated from the body surface of a mason bee (Osmia cornifrons)–derived Streptomyces sp. OC1611-8A. Its structure is identified by high-resolution electrospray ionization mass spectrometry data and nuclear magnetic resonance spectroscopic analysis. The absolute configuration of cornifronone was determined by electronic circular dichroism spectra

Amorphous MoS2 spheres with diameters ranging from 150 nm to 1.5 μm are successfully prepared following a reliable one-pot hydrothermal route using a homemade autoclave and inexpensive reactants, at a low temperature (160 °C) and a short reaction time (12 h). The obtained material is comprehensively characterized by X-ray diffraction, scanning-electron microscopy, energy-dispersive X-ray spectroscopy

A new luminescent, cationic, heteroleptic, four-coordinate Cu(I)–N-heterocyclic carbene complex [Cu(Br-Pyim)(POP)](PF6) is successfully prepared and characterized, where Br-Pyim and POP are 1-(6-bromopyridin-2-yl)imidazole-3-benzyl-2-ylidene and bis[2-(diphenylphosphino)phenyl]ether, respectively. Its detailed structure is determined by single-crystal X-ray analysis. It exists as a crystalline powder

Deoxygenative chlorination of carbonyl compounds using the HMe2SiCl/FeCl3/EtOAc and HMeSiCl2/FeCl3/EtOAc systems has been systemically investigated. The HMe2SiCl-FeCl3 system showed the advantages of good substrate applicability, mild reaction conditions, simple operation, low cost, and easy availability of raw materials. Also, it provided a simple and efficient synthesis route for carbonyl deoxychlorination