Distereoselective one-pot synthesis of pyrimidopyrimidines using sulfated tin oxide as a reusable catalyst： An extension of Biginelli-type reaction

The Biginelli-type compounds 4,5,8a-triarylhexahydropyrimido[4,5-d]pyrimidine-2,7（1H,3H）-diones were synthesized by a one-pot three-component reaction using sulfated tin oxide as a reusable catalyst. This method has the advantages of high yields, short reaction time, simple starting materials and reusability of catalyst for several times.     

2,4,6-Tris(4-iodophenoxy)-1,3,5-triazine as a new recyclable “iodoarene” for in situ generation of hypervalent iodine(III) reagent for α-tosyloxylation of enolizable ketones

The synthesis of 2,4,6-tris[(4-iodo)phenoxy)]-1,3,5-triazine 6, as a new recyclable nonpolymeric analogue of iodobenzene is achieved using the reaction of 2,4,6-trichloro-1,3,5-triazine with 4-iodophenol in the presence of KOH. The application of 6 as a recyclable ‘iodoarene’ is demonstrated for α-tosyloxylation of enolizable ketones via in situ generation of hypervalent iodine(III) species using PTSA and MCPBA as the terminal oxidant. The recyclability of the reagent 6 was possible owing to the facile recovery and reuse from the reaction mixture due to its near insolubility in methanol.     

Crystal structures of the pyrazinamide–p‐aminobenzoic acid (1/1) cocrystal and the transamidation reaction product 4‐(pyrazine‐2‐carboxamido)benzoic acid in the molten state

The synthesis of pharmaceutical cocrystals is a strategy to enhance the performance of active pharmaceutical ingredients (APIs) without affecting their therapeutic efficiency. The 1:1 pharmaceutical cocrystal of the antituberculosis drug pyrazinamide (PZA) and the cocrystal former p‐aminobenzoic acid (p‐ABA), C₇H₇NO₂·C₅H₅N₃O, (1), was synthesized successfully and characterized by relevant solid‐state characterization methods. The cocrystal crystallizes in the monoclinic space group P2₁/n containing one molecule of each component. Both molecules associate via intermolecular O—H...O and N—H...O hydrogen bonds [O...O = 2.6102 (15) Å and O—H...O = 168.3 (19)°; N...O = 2.9259 (18) Å and N—H...O = 167.7 (16)°] to generate a dimeric acid–amide synthon. Neighbouring dimers are linked centrosymmetrically through N—H...O interactions [N...O = 3.1201 (18) Å and N—H...O = 136.9 (14)°] to form a tetrameric assembly supplemented by C—H...N interactions [C...N = 3.5277 (19) Å and C—H...N = 147°]. Linking of these tetrameric assemblies through N—H...O [N...O = 3.3026 (19) Å and N—H...O = 143.1 (17)°], N—H...N [N...N = 3.221 (2) Å and N—H...N = 177.9 (17)°] and C—H...O [C...O = 3.5354 (18) Å and C—H...O = 152°] interactions creates the two‐dimensional packing. Recrystallization of the cocrystals from the molten state revealed the formation of 4‐(pyrazine‐2‐carboxamido)benzoic acid, C₁₂H₉N₃O₃, (2), through a transamidation reaction between PZA and p‐ABA. Carboxamide (2) crystallizes in the triclinic space group P with one molecule in the asymmetric unit. Molecules of (2) form a centrosymmetric dimeric homosynthon through an acid–acid O—H...O hydrogen bond [O...O = 2.666 (3) Å and O—H...O = 178 (4)°]. Neighbouring assemblies are connected centrosymmetrically via a C—H...N interaction [C...N = 3.365 (3) Å and C—H...N = 142°] engaging the pyrazine groups to generate a linear chain. Adjacent chains are connected loosely via C—H...O interactions [C...O = 3.212 (3) Å and C—H...O = 149°] to generate a two‐dimensional sheet structure. Closely associated two‐dimensional sheets in both compounds are stacked via aromatic π‐stacking interactions engaging the pyrazine and benzene rings to create a three‐dimensional multi‐stack structure.     

Deposition of copper iodide thin films by chemical bath deposition (CBD) and successive ionic layer adsorption and reaction (SILAR) methods

In this paper, we report structural, morphological, electrical studies of copper iodide (CuI) thin films deposited onto glass substrates by chemical bath deposition (CBD) and successive ionic layer adsorption and reaction (SILAR) methods. CuI thin films were characterized for their structural, morphological and wettability studies by means of X-ray diffraction (XRD), FT-Raman spectroscopy, scanning electron microscopy (SEM), optical absorption, and contact angle measurement methods. Thickness of thin films was 1 ± 0.1 μm measured by gravimetric weight difference method. The CuI thin films were nanocrystalline, with average crystal size of ～60 nm. The FT-IR study confirmed the formation of CuI on the substrate surface. SEM images revealed the compact and cube like structure for CuI thin films deposited by CBD and SILAR methods, respectively. Optical absorption study revealed optical energy gaps as 2.3 and 3.0 eV for CBD and SILAR methods, respectively. Wettability study indicated that CuI thin films deposited by SILAR method are more hydrophobic as compared to CBD method.     

Ni<Superscript>2+</Superscript>-substituted Mg–Cu–Zn ferrites: a colloidal approach of tuning structural and electromagnetic properties

A robust synthesis approach to Ni²⁺-substituted Mg_0.25-xNi _x Cu_0.25Zn_0.5Fe₂O₄ (0?≤?x?≤?0.25?mol.) ferrimagnetic oxides using citrate assisted sol–gel process is reported. The route utilizes simple metal nitrate precursors in aqueous solution, thus eliminating the need for organometallic precursors. Citric acid acts as a fuel for the combustion reaction and forms stable complexes with metal ions preventing the precipitation of hydroxilated compounds to yield the composite ferrite structure by auto-combustion process. The XRD signatures, especially (3 1 1) plane, confirmed the formation of spinel structure. The linear growth of lattice constant from 8.385 to 8.409?Å was observed by Ni²⁺ substitution from 0 to 0.25. The dense microstructure is observed with the average grain size of 0.42–2.18?µm. The transport properties revealed the semiconducting behavior of as-prepared ferrite material, with an increase in the DC-electrical resistivity by the incorporation of nickel. The magnetic properties viz. initial permeability (µ_i) and magnetic moment (n_B) are explained, based on the deviation in saturation magnetization (M_s), anisotropy constant (K₁)_, density values, and exchange interactions. Furthermore, the effect of adding Ni²⁺ on the Curie temperature, frequency-dependent dielectric properties of the ferrite material are also discussed.

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含油岩心显微荧光成像光谱研究

发展了一种显微荧光光谱成像技术,并将其应用于天然岩心进行显微荧光成像光谱研究。利用这种技术同时采集含油岩心表面的荧光光谱信息和空间信息．并对获得的光谱图像给予光谱学和地质学解释。结果表明,不但能显示岩心形貌和组分的大致趋势,而且能揭示其精细细节．为石油地质研究提供了一种新方法,为今后的石油勘探开发工作提供了一种先进的指导手段。     

Multiple 3D- and 2D-quantitative structure–activity relationship models (QSAR), theoretical study and molecular modeling to identify structural requirements of imidazopyridine analogues as anti-infective agents against tuberculosis

Structural Chemistry - Tuberculosis (TB), an infectious remains a global health burden till date. Considering immense importance of theoretical tools in computer aided-drug designing, the current...     

Poly(methyl methacrylate)-Assisted Exfoliation of Graphite and Its Use in Acrylonitrile-Butadiene-Styrene Composites

One of the applications of graphene in which its scalable production is of utmost importance is the development of polymer composites. Among the techniques used to produce graphene flakes, the liquid-phase exfoliation (LPE) of graphite stands out due to its versatility and scalability. However, solvents suitable for the LPE process are generally toxic and have a high boiling point, making the processing challenging. The use of low boiling point solvents could be convenient for the processing, due to the easiness of their removal. In this study, the use of poly(methyl methacrylate) (PMMA) as a stabilizing agent is proposed for the production of graphene flakes in a low boiling point solvent, that is, acetone. The graphene dispersions produced in the mixture acetone-PMMA have higher concentration, +175 %, and contain a higher percentage of few-layer graphene flakes (<5 layers), that is, +60 %, compared to the dispersions prepared in acetone. The as-produced graphene dispersions are used to develop graphene/acrylonitrile-butadiene-styrene composites. The mechanical properties of the pristine polymer are improved, that is, +22 % in the Young's modulus, by adding 0.01 wt. % of graphene flakes. Moreover, a decrease of ≈20 % in the oxygen permeability is obtained by using 0.1 wt. % of graphene flakes filler, compared to the unloaded matrix.     

Analysis of a shielded TE011 mode composite dielectric resonator for stable frequency reference

Analysis of a TE₀₁₁ mode composite sapphire-rutile dielectric resonator has been carried out to study the temperature variation of resonance frequency, close to the Cs atomic clock hyperfine frequency of 9.192 GHz. The complementary behavior of dielectric permittivity with temperature of the composite has been exploited to obtain the desired turning point in the resonant frequency. The frequency of the composite structure is found to be independent of the shield diameter beyond four times the puck diameter.