scholarly journals High Yielding, One-Pot Synthesis of Bis(1H-indazol-1-yl)methane Catalyzed by 3d-Metal Salts

Reactions ◽  
2022 ◽  
Vol 3 (1) ◽  
pp. 59-69
Author(s):  
Natalie M. Lind ◽  
Natalie S. Joe ◽  
Brian S. Newell ◽  
Aimee M. Morris

Synthetic access to poly(indazolyl)methanes has limited their study despite their structural similarity to the highly investigated chelating poly(pyrazolyl)methanes and their potentially important indazole moiety. Herein is presented a high yielding, one-pot synthesis for the 3d-metal catalyzed formation of bis(1H-indazol-1-yl)methane from 1H-indazole utilizing dimethylsulfoxide as the methylene source. Complete characterization of bis(1H-indazol-1-yl)methane is given with 1H and 13C NMR, UV/Vis, FTIR, high resolution mass spectrometry and for the first time, single crystal X-ray diffraction. This simple, inexpensive pathway to yield exclusively bis(1H-indazol-1-yl)methane provides synthetic access to further investigate the coordination and potential applications of the family of bis(indazolyl)methanes.

2018 ◽  
Vol 22 (09n10) ◽  
pp. 814-820
Author(s):  
Yingying Jia ◽  
Ling Xu ◽  
Bangshao Yin ◽  
Mingbo Zhou ◽  
Jianxin Song

Beginning with 5,10,15-triarylporphyrin-nickel complex, five meso-to-meso directly linked porphyrin-diazaporphyrin triads were successfully prepared for the first time through a series of reactions including formylation via Vilsmeier–Haack reaction, condensation with pyrrole, bromination with [Formula: see text]-Bromosuccinimide (NBS), oxidation with 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ), metal-templated cyclization of dibromodipyrrin-metal complexes with NaN[Formula: see text] and demetalization. All these triads were comprehensively characterized by [Formula: see text]H NMR, high-resolution mass spectrometry and UV-vis absorption. In addition, the structure of compound 6Ni was unambiguously determined by X-ray diffraction analysis, which showed that the two dihedral angles are both 86.65 (4)[Formula: see text] between each mean plane of porphyrin and that of central diazaporphyrin The UV-vis absorption spectra disclosed that the longest wavelengths of Soret bands and Q bands for these triads were observed at 429 and 642 nm, respectively. In contrast to diazaporphyrin-porphyrin dyads, diazaporphyrin dimers and diazaporphyrin monomers reported previously the molar extinction coefficients, particularly for triad 8Ni are much higher.


2019 ◽  
Vol 118 ◽  
pp. 01059
Author(s):  
Xiaoyang Li ◽  
Genwang Zhang ◽  
Binwei Wang ◽  
Tan Lin ◽  
Guo Wang ◽  
...  

One-pot synthesis of polyaniline/Fe3O4 nanocomposite in 1-methyl-3-alkylcarboxylic acid imidazolium chloride ([CMMIm]Cl) ionic liquid (IL) was introduced for the first time in this work. Transmission electron microscopy (TEM), X-ray diffraction (XRD), four probes method and vibrating sample magnetometer (VSM) were used to explore the influence of IL on the structure, conductivity and magnetic properties of polyaniline/Fe3O4 composite. Compared with Fe3O4 particles prepared in water, the results show that Fe3O4 particles prepare in imidazolium-based ionic liquid were more regular in shape and dispersed uniformly. So the Fe3O4 nanoparticles prepared in IL can easier serve as cores to form the polyaniline/Fe3O4 nanocomposite via in situ chemical oxidative polymerization of aniline molecule. The saturation magnetization of polyaniline/Fe3O4 nanocomposite prepared in ionic liquid shows about 2 times higher than polyaniline/Fe3O4 composite prepared in water. And the conductivities of PANI/Fe3O4 composite prepared in IL decreased and the saturated magnetization increased with the increasing amount of Fe3O4.


2016 ◽  
Vol 40 (3) ◽  
pp. 2541-2546 ◽  
Author(s):  
Amey Nimkar, M. M. V. Ramana ◽  
Rahul Betkar ◽  
Prasanna Ranade ◽  
Balaji Mundhe

Pyrimidine derivatives were synthesized in one pot using a novel heterogeneous reusable catalyst, and complete characterization of catalyst was performed.


2020 ◽  
Vol 23 (23) ◽  
pp. 2626-2634
Author(s):  
Saiedeh Kamalifar ◽  
Hamzeh Kiyani

: An efficient and facial one-pot synthesis of 4-aryl-3,4-dihydrobenzo[g]quinoline- 2,5,10(1H)-triones was developed for the first time. The process proceeded via the three-component cyclocondensation of 2-amino-1,4-naphthoquinone with Meldrum’s acid and substituted benzaldehydes under green conditions. The fused 3,4-dihydropyridin-2(1H)- one-ring naphthoquinones have been synthesized with good to high yields in refluxing ethanol as a green reaction medium. This protocol is simple and effective as well as does not involve the assistance of the catalyst, additive, or hazardous solvents.


RSC Advances ◽  
2015 ◽  
Vol 5 (61) ◽  
pp. 49295-49300 ◽  
Author(s):  
Handan Pamuk ◽  
Burak Aday ◽  
Fatih Şen ◽  
Muharrem Kaya

Pt NPs@GO has been used for the first time for synthesizing acridinedione from dimedone, aromatic aldehydes and various amines as a catalyst.


Synlett ◽  
2018 ◽  
Vol 29 (12) ◽  
pp. 1589-1592 ◽  
Author(s):  
Abolfazl Olyaei ◽  
Mahnaz Saraei ◽  
Reyhaneh Khoeiniha

A high-yielding cyclocondensation of 4-hydroxycoumarin, phenylglyoxal monohydrate, and heteroarylamines proceeds without catalysis, which gives novel functionalized furo[3,2-c]coumarins and heteroarylamino alkylation of coumarin products in acetonitrile under reflux, is reported for the first time. This tandem process involves sequentially an aldol condensation, Michael addition, a ring closure, and dehydration reaction.


2011 ◽  
Vol 480-481 ◽  
pp. 1065-1069
Author(s):  
Bin Liu ◽  
Lin Wang ◽  
Yin Zhong Bu ◽  
Sheng Rong Yang ◽  
Jin Qing Wang

Titanium (Ti) and its alloys have been applied in orthopedics as one of the most popular biomedical metallic implant materials. In this work, to enhance the bioactivity, the surface of Ti alloy pre-modified by silane coupling agent and glutaraldehyde was covalently grafted with chitosan (CS) via biochemical multistep self-assembled method. Then, for the first time, the achieved surface was further immobilized with casein phosphopeptides (CPP), which are one group of bioactive peptides released from caseins in the digestive tract and can facilitate the calcium adsorption and usage, to form CS-CPP biocomposite coatings. The structure and composition of the fabricated coatings were characterized by X-ray photoelectron spectroscopy (XPS), attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR) and atomic force microscopy (AFM). As the experimental results indicated, multi-step assembly was successfully performed, and the CS and CPP were assembled onto the Ti alloy surface orderly. It is anticipated that the Ti alloys modified by CS-CPP biocomposite coatings will find potential applications as implant materials in biomedical fields.


1996 ◽  
Vol 459 ◽  
Author(s):  
E. Ching-Prado ◽  
W. Pérez ◽  
A. Reynés-Figueroa ◽  
R. S. Katiyar ◽  
D. Ravichandran ◽  
...  

ABSTRACTThin films of SrBi2Nb2O9 (SBN) with thicknesses of 0.1, 0.2, and 0.4 μ were grown by Sol-gel technique on silicon, and annealed at 650°C. The SBN films were investigated by Raman scatering for the first time. Raman spectra in some of the samples present bands around 60, 167, 196, 222, 302, 451, 560, 771, 837, and 863 cm−1, which correspond to the SBN formation. The study indicates that the films are inhomogeneous, and only in samples with thicknesses 0.4 μ the SBN material was found in some places. The prominent Raman band around 870 cm−1, which is the A1g mode of the orthorhombic symmetry, is assigned to the symmetric stretching of the NbO6 octahedrals. The frequency of this band is found to shift in different places in the same sample, as well as from sample to sample. The frequency shifts and the width of the Raman bands are discussed in term of ions in non-equilibrium positions. FT-IR spectra reveal a sharp peak at 1260 cm−1, and two broad bands around 995 and 772 cm−1. The bandwidths of the latter two bands are believed to be associated with the presence of a high degree of defects in the films. The experimental results of the SBN films are compared with those obtained in SBT (T=Ta) films. X-ray diffraction and SEM techniques are also used for the structural characterization.


Molecules ◽  
2021 ◽  
Vol 26 (3) ◽  
pp. 518
Author(s):  
Somaye Akbari ◽  
Addie Bahi ◽  
Ali Farahani ◽  
Abbas S. Milani ◽  
Frank Ko

Blending lignin as the second most abundant polymer in Nature with nanostructured compounds such as dendritic polymers can not only add value to lignin, but also increase its application in various fields. In this study, softwood Kraft lignin/polyamidoamine dendritic polymer (PAMAM) blends were fabricated by the solution electrospinning to produce bead-free nanofiber mats for the first time. The mats were characterized through scanning electron microscopy, Fourier transform infrared (FTIR) spectroscopy, zeta potential, and thermogravimetry analyses. The chemical intermolecular interactions between the lignin functional groups and abundant amino groups in the PAMAM were verified by FTIR and viscosity measurements. These interactions proved to enhance the mechanical and thermal characteristics of the lignin/PAMAM mats, suggesting their potential applications e.g. in membranes, filtration, controlled release drug delivery, among others.


2018 ◽  
Vol 82 (5) ◽  
pp. 1049-1055 ◽  
Author(s):  
Daniel Atencio ◽  
Marcelo B. Andrade ◽  
Luca Bindi ◽  
Paola Bonazzi ◽  
Matteo Zoppi ◽  
...  

ABSTRACTThis study presents a complete characterization of kenoplumbomicrolite, (Pb,□)2Ta2O6[□,(OH),O], occurring in an amazonite pegmatite from Ploskaya Mountain, Western Keivy Massif, Kola Peninsula, Murmanskaja Oblast, Northern Region, Russia.Kenoplumbomicrolite occurs in yellowish brown octahedral, cuboctahedral and massive crystals, up to 20 cm, has a white streak, a greasy lustre and is translucent. The Mohs hardness is ~6. Attempts to measure density (7.310–7.832 g/cm3) were affected by the ubiquitous presence of uraninite inclusions. Reflectance values were measured in air and immersed in oil. Kenoplumbocrolite is optically isotropic. The empirical formula is (Pb1.30□0.30Ca0.29Na0.08U0.03)Σ2.00(Ta0.82Nb0.62Si0.23Sn4+0.15Ti0.07Fe3+0.10Al0.01)Σ2.00O6[□0.52(OH)0.25O0.23]Σ1.00 (from the crystal used for the structural study) and (Pb1.33□0.66Mn0.01)Σ2.00(Ta0.87Nb0.72Sn4+0.18Fe3+0.11W0.08Ti0.04)Σ2.00O6[□0.80(OH)0.10O0.10]Σ1.00 (average including additional fragments). The mineral is cubic, space group Fd$\overline 3 $m. The unit-cell parameters refined from powder X-ray diffraction data are a = 10.575(2) Å and V = 1182.6(8) Å3, which are in accord with those obtained previously from a single crystal of a = 10.571(1) Å, V = 1181.3(2) Å3 and Z = 8. The mineral description and its name have been approved by the Commission on New Minerals, Nomenclature and Classification of the International Mineralogical Association (IMA2015-007a).


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