An efficient method for the oxidative transformation of thioamides and thioketones to their oxygen analogues with singlet oxygen is reported. Singlet oxygen was produced in situ from the fragmentation of the trans-5-hydroperoxy-3,5-dimethyl-1,2-dioxolane-3-yl ethaneperoxate in the presence of KOH, and it has been explored as an effective oxidant for oxidative desulfurization of thioamides and thioketones. This protocol provides amides and ketones in excellent yields (80–90%) at room temperature under mild conditions. The thioamides reacted very well with this reagent system. The conjugation of neighboring NH and C=S groups appears to enhance yields for thioamides. Further investigation showed that this reagent system is also an efficient system for deprotection of thionoesters to esters.
Thiosalicylate anions are known for their complexing capacity towards a wide range of transition metals. We have used this important sulfur-containing anion to synthesize the task-specific ionic liquid dioctylimidazolium thiosalicylate [DOIM] [TS] via ion exchange method in two steps. For characterization of [DOIM] [TS] we have used, electron spray ionization mass spectroscopy (ESIMS), nuclear magnetic resonance (NMR), infrared spectroscopy (IR), and thermal gravimetric analysis (TGA). The sulfur-containing IL was investigated for the removal of heavy metals (Cr3+, Mn2+, Fe2+, Co2+, Ni2+, Cu2+) from their aqueous solutions. The extraction efficiencies were determined through atomic absorption spectroscopy.
The crystal structure of the title solvated coordination compound, [Co (SCN)4 (BtaH)2]·(BtaH)2.6(H2O), consists of discrete complexes in which the Co2+ cations are sixfold coordinated by four N-bonded thiocyanate anions and two 1-H benzotriazolium molecules to generate distorted trans-CoN6 octahedra. The discrete entities are each connected by three solvate molecules into chains via strong O—H···N hydrogen bonds. These chains are further linked by additional O—H···N, N—H···O, N—H···S, O—H···S and O—H···O hydrogen bonds into a three-dimensional network. Within this network, channels are formed that propagate along the c-axis direction and embed additional acetonitrile solvent molecules that are hydrogen-bonded to the network. In addition, density functional theory (DFT) calculations using the M06-2X/gen method were used to study the system's electronic properties. Interestingly, molecular docking and topological analyses were performed on compounds against various target anti-inflammatory receptors to investigate which targets exhibit the best binding affinities and hydrogen-bonding interactions. Done. As a result, it exhibits excellent anti-inflammatory activity, making it a suitable drug candidate for inflammatory diseases.
Three novel organotellurium (IV) derivatives of diphenyldithiocarbamate, C4H8Te[(CS2) N(C6H5)2]2 (1), (C2H5)2Te[(CS2) N(C6H5)2]2 (2), and C4H7(CH3)Te[(CS2) N(C6H5)2]2 (3) have been synthesized by the reaction of sodium salt of diphenyl dithiocarbamate with C4H8TeI2, (C2H5)2TeI2, and C4H7(CH3)TeI2 respectively. The synthesized compounds 1–3 were characterized by elemental analysis, IR, 1H NMR, and 13C{1H} NMR spectroscopic studies. The antimicrobial efficacy of compounds 1–3 was examined against selected bacterial and fungal strains using broth microdilution and disc diffusion methods. Penicillin and amphotericin B were used as a positive control for bacterial and fungal strains respectively. The highest activity against bacterial strains was shown by compound 3 while against the fungal strain compound 1 showed the highest activity with a MIC value of 6.25 µg/ml. However, all compounds showed high to moderate antimicrobial activity.
Two solvent-controlled Cd(II) compounds, formulated as {[Cd2(Htdc)4(µ-imyp)(H2O)4]} (1), [Cd2(µ2-tdc)2(µ-imyp)(DMF)2(H2O)2]n (2) (H2tdc= 2,5-thiophenedicarboxylic acid, imyp = 4-imidazol-1-yl-pyridine and DMF = N,N-dimethylformamide) have been synthesized by reactions of Cd(NO3)2·4H2O and H2tdc with imyp in different solvents, respectively. Both compounds were then characterized by single-crystal X-ray diffraction and other physicochemical methods. In 1, partially deprotonated Htdc− anion as terminal ligand and µ-imyp ligand connect Cd2+ ions to generate a discrete structure. In 2, completely deprotonated µ2 – tdc2− anions and µ-imyp ligand link Cd2+ ions into a 1D double chain structure. Both compounds display 3D supramolecular structures through hydrogen bonding interactions. The results provided interesting insights into solvent effects on the structural formation of compounds 1 and 2. In addition, the solid-state photoluminescent properties of compounds 1 and 2 were also investigated.
Two solvent-controlled Cd(II) compounds have been synthesized by reactions of Cd(NO3)2·4H2O and 2,5-thiophenedicarboxylic acid with 4-imidazol-1-yl-pyridine in the different solvents. One compound is a discrete structure, while the other compound has a 1D double chain structure. The results provided interesting insights into solvent effects on the structural formation of compounds.
Thiazolidines (TZs) are a significant class of heterocyclic compounds displaying several pharmaceutical, and biological activities. Because of our interest in the chemistry and biology of heterocycles, with the exploitation of ionic liquids (ILs) in organic transformations, herein, the recent preparative developments for TZs in ILs are deliberated wherein ILs play the dual role of solvent and catalysts. The preparation of various types of TZs, namely 1,3-thiazolidine-4-ones bearing azo-linkage, spiro-[indole-thiazolidine]-2,4’-diones, 2-(2-oxo-chromenyl)-3-thiazolidinones, 2-pyrazolo-thiazolidineones, 2-imino-thiazolidine, and pyridine-based 5-amino-2-oxo-thiazolo[4,5-b] pyridine-6-carbonitriles has been described using various ILs. This review aims at the synthesis advancement in the assembly of TZs in ILs during 2012–2023, under various conditions such as reflux, stirring, solvent-free or microwave, and ultrasound irradiation conditions. Devoid of vapor pressure, and being recyclable, ILs are relatively eco-friendly, especially for inherently sustainable multi-component reactions (MCRs) that are atom-economic and are endowed with waste reduction attributes in terms of fewer manipulations.
In this work, tetrahydrobenzo[a]xanthene-11-ones are effectively synthesized without the need for solvents and in an environmentally safe manner by the use of indium sulfide (In2S3) nanoparticle as a catalyst. Indium sulfide (In2S3) nanoparticles were synthesized by the hydrothermal method, and X-ray diffraction pattern (XRD), energy-dispersive X-ray spectroscopy (EDS), scanning electron microscopy (SEM), and transition electron microscopy (TEM) were among the techniques used to characterize indium sulfide (In2S3) nanoparticles. The synthesis of tetrahydrobenzo[a]xanthene-11-ones was achieved in a single pot using a three-component reaction involving β-naphthol, dimedone, and aryl aldehyde. The resultant indium sulfide (In2S3) nanoparticles were produced without the need for a solvent and exhibited remarkable yields, as well as quick reaction times and reusable catalysts.
This study introduces a simple, cost-effective, and rapid bismuth electrode-square-wave voltammetry method for determining the total sulfur content in automotive gasoline. Optimal conditions for the developed electrode, including various Bi ion concentrations, deposition times, and potentials, were established on a glassy carbon electrode. The results demonstrated that the highest response was achieved when the bismuth electrode was placed in an acetate buffer and a methanol:toluene (1:1 v/v) solvent. The method was validated with and without a 30-second electro-preconcentration step. The voltammetric method in conjunction with the preconcentration step exhibited a sensitivity of 571.81 nA mg L−1, a limit of detection (LOD) of 0.02 mg L−1, and a limit of quantification (LOQ) of 0.08 mg L−1. Without the preconcentration step, the method yielded a sensitivity of 421.89 nA mg L−1, an LOD of 0.03 mg L−1, and an LOQ of 0.11 mg L−1. The developed method was applied to quantify commercial fuel samples. The results showed that the electrochemical technique yielded a similar total sulfur content to that measured by the standard ASTM D2622 method, with an error of less than 7.5%. Moreover, the method proposed in this study had lower LOD and LOQ limits, meeting the EURO5 and EURO6 regulations.