scholarly journals Synthesis of 3-Aryl-ortho-carboranes with Sensitive Functional Groups

Molecules ◽  
2021 ◽  
Vol 26 (23) ◽  
pp. 7297
Author(s):  
Sergey A. Anufriev ◽  
Akim V. Shmal’ko ◽  
Kyrill Yu. Suponitsky ◽  
Igor B. Sivaev
Keyword(s):  
Functional Groups ◽  
Intramolecular Hydrogen Bonding ◽  
X Ray Diffraction ◽  
One Pot ◽  
X Ray ◽  
The One ◽  
Intramolecular Hydrogen ◽  
Solid State Structures ◽  
Derivatives Of

A simple and efficient method was developed for the one-pot synthesis of 3-aryl derivatives of ortho-carborane with sensitive functional groups using 3-iodo-ortho-carborane and aryl zinc bromides that were generated in situ. A series of 3-aryl-ortho-carboranes, including those containing nitrile and ester groups, 3-RC6H4-1,2-C2B10H11 (R = p-Me, p-NMe2, p-OCH2OMe, p-OMe, o-CN, p-CN, o-COOEt, m-COOEt, p-COOEt) was synthesized using this approach. The solid-state structures of 3-RC6H4-1,2-C2B10H11 (R = p-OMe, o-CN, and p-CN) were determined by single crystal X-ray diffraction. The intramolecular hydrogen bonding involving the ortho-substituents of the aryl ring and the CH and BH groups of carborane was discussed.

scholarly journals One-Pot Synthesis of B-Aryl Carboranes with Sensitive Functional Groups Using Sequential Cobalt- and Palladium-Catalyzed Reactions

Catalysts ◽  
2020 ◽  
Vol 10 (11) ◽  
pp. 1348
Author(s):  
Sergey A. Anufriev ◽  
Akim V. Shmal’ko ◽  
Kyrill Yu. Suponitsky ◽  
Igor B. Sivaev
Keyword(s):  
Functional Groups ◽  
X Ray Diffraction ◽  
One Pot ◽  
One Pot Synthesis ◽  
Palladium Catalyzed ◽  
Catalyzed Reactions ◽  
The One ◽  
Solid State Structures ◽  
Derivatives Of

The simple and efficient method was developed for the one-pot synthesis of B-substituted aryl derivatives of ortho-carborane with functional groups sensitive to organolithium and organomagnesium reagents using 9-iodo-ortho-carborane and generated in situ organozinc compounds. The method proposed was used to prepare a series of 9-aryl-ortho-carboranes, including those containing nitrile and ester groups, 9-RC6H4-1,2-C2B10H11 (R = p-Me, p-NMe2, p-OCH2OMe, o-OMe, p-OMe, o-CN, p-CN, o-COOEt, m-COOEt, and p-COOEt). It was demonstrated that the same approach can be used for synthesis of diaryl derivatives of ortho-carborane 9,12-(RC6H4)2-1,2-C2B10H10 (R = H, p-Me). The solid-state structures of 9-RC6H4-1,2-C2B10H11 (R = p-NMe2, p-OCH2OMe, o-OMe, o-CN, p-CN, m-COOEt, and p-COOEt) and 9,12-(p-MeC6H4)2-1,2-C2B10H10 were determined by single crystal X-ray diffraction.

scholarly journals Time-resolved XRD experiments for a fine description of mechanisms induced during reactive sintering

2005 ◽  
Vol 37 (1) ◽  
pp. 27-34 ◽  
Author(s):  
S. Paris ◽  
E. Gaffet ◽  
D. Vrel ◽  
D. Thiaudiere ◽  
M. Gailhanou ◽  
...  
Keyword(s):  
Reactive Sintering ◽  
X Ray Diffraction ◽  
Reaction Parameters ◽  
Time Resolved ◽  
X Ray ◽  
Synthesis Conditions ◽  
Nanostructure Materials ◽  
Synchrotron Beam ◽  
The One

The control of Mechanically Activated Field Activated Pressure Assisted Synthesis hereafter called the MAFAPAS process is the main objective to be achieved for producing nanostructure materials with a controlled consolidation level. Consequently, it was essential to develop characterization tools "in situ" such as the Time Resolved X-ray Diffraction (TRXRD), with an X-ray synchrotron beam (H10, LURE Orsay) coupled to an infrared thermography to study simultaneously structural transformations and thermal evolutions. From the 2003 experiments, we took the opportunity to modify the sample-holder in order to reproduce the better synthesis conditions of the MAFAPAS process, but without the consolidation step. The versatility of the setup has been proved and could even be enhanced by the design of new sample holders. In addition, this work clearly shows that this equipment will allow, on the one hand, to make progress of the understanding of MAFAPAS mechanisms and, on the other hand, to adjust reaction parameters (mechanical activation and combustion synthesis) for producing many materials with an expected microstructure.

scholarly journals Bis(dicarbollide) Complexes of Transition Metals as a Platform for Molecular Switches. Study of Complexation of 8,8′-Bis(methylsulfanyl) Derivatives of Cobalt and Iron Bis(dicarbollides)

Molecules ◽  
2020 ◽  
Vol 25 (23) ◽  
pp. 5745
Author(s):  
Sergey A. Anufriev ◽  
Sergey V. Timofeev ◽  
Alexei A. Anisimov ◽  
Kyrill Yu. Suponitsky ◽  
Igor B. Sivaev
Keyword(s):  
Solid State ◽  
Transition Metal ◽  
Molecular Switches ◽  
X Ray Diffraction ◽  
Chelate Complexes ◽  
X Ray ◽  
Complexes Of Transition Metals ◽  
Silver Palladium ◽  
Solid State Structures ◽  
Derivatives Of

Complexation of the 8,8′-bis(methylsulfanyl) derivatives of cobalt and iron bis(dicarbollides) [8,8′-(MeS)2-3,3′-M(1,2-C2B9H10)2]− (M = Co, Fe) with copper, silver, palladium and rhodium leads to the formation of the corresponding chelate complexes, which is accompanied by a transition from the transoid to the cisoid conformation of the bis(dicarbollide) complex. This transition is reversible and can be used in design of coordination-driven molecular switches based on transition metal bis(dicarbollide) complexes. The solid-state structures of {(Ph3P)ClPd[8,8′- (MeS)2-3,3′-Co(1,2-C2B9H10)2-κ2-S,S′]} and {(COD)Rh[8,8′-(MeS)2-3,3′-Co(1,2-C2B9H10)2-κ2-S,S′]} were determined by single crystal X-ray diffraction.

5,6,7,8-Tetrahydronaphthalen-1-amine as Precursor for Thiazolidi­nones and Benzothiazepinones: Synthesis and Atropisomeric Relationship

Synthesis ◽  
2017 ◽  
Vol 49 (23) ◽  
pp. 5167-5175 ◽  
Author(s):  
Bruna Drawanz ◽  
Georgia Zimmer ◽  
Leticia Rodrigues ◽  
Andressa Nörnberg ◽  
Manfredo Hörner ◽  
...  
Keyword(s):  
Small Difference ◽  
Mercaptoacetic Acid ◽  
X Ray Diffraction ◽  
Ring Plane ◽  
One Pot ◽  
X Ray ◽  
Nmr Techniques ◽  
The One ◽  
Electron Donating Groups ◽  
Weak Electron

The one-pot reaction of 5,6,7,8-tetrahydronaphthalen-1-amine, mercaptoacetic acid, and arenealdehydes having strong and weak electron-withdrawing groups gave the corresponding 1,3-thiazolidin-4-ones (47–70%). When arenealdehydes bearing strong and weak electron-donating groups were used as precursors, the 1,4-benzothiazepin-2-ones were obtained (30–72%) by p-TsOH catalysis. All compounds are unknown and were characterized by GC-MS and NMR techniques, and available crystals by X-ray diffraction studies. The atropisomerism phenomenon was observed in several 1,3-thiazolidin-4-ones as confirmed by VTNMR method. The Tc was established as 332 K and the energy required for the interconversion of one atrop­isomer into another is around 16.8 kcal·mol–1. Chemical quantum calculation and NOESY displayed that more stable isomer has the tetrahydro­naphthalene portion below the five-ring plane. Only a small difference between isomers (–0.21 to –0.84 kcal·mol–1) was observed by calculated energy.

scholarly journals One-Pot Access to Diverse Functionalized Pyran Annulated Heterocyclic Systems Using SCMNPs@BPy-SO3H as a Novel Magnetic Nanocatalyst

2020 ◽  
Vol 15 (2) ◽  
pp. 348-366 ◽  
Author(s):  
Ke Chen ◽  
Guangzu He ◽  
Qiong Tang ◽  
Qahtan A.Yousif
Keyword(s):  
Magnetic Field ◽  
Reaction Times ◽  
Vibrating Sample Magnetometry ◽  
X Ray Diffraction ◽  
Magnetic Nanocatalyst ◽  
Permanent Magnetic Field ◽  
One Pot ◽  
X Ray ◽  
The One ◽  
Scanning Electron

The SCMNPs@BPy-SO3H catalyst was prepared and characterized using Fourier Transform Infrared Spectroscopy (FTIR), Thermogravimetric Analysis (TGA), Vibrating Sample Magnetometry (VSM), Energy Dispersive X-ray Spectroscopy (EDX), X-ray Diffraction (XRD), and Scanning Electron Microscopy (SEM). Afterwards, its capability was efficiently used to promote the one-pot, three-component synthesis of pyrano[2,3-c]pyrazole and 2-amino-3-cyano-pyrano[3,2-c]chromen-5(4H)-one derivatives. The strategy resulted in the desired products with excellent yields and short reaction times. The SCMNPs@BPy-SO3H catalyst was readily recovered using a permanent magnetic field and it was reused in six runs with a slight decrease in catalytic activity. Copyright © 2020 BCREC Group. All rights reserved 

scholarly journals Poly (N-Methyl Aniline)-Li Nanocomposite as an Electrolyte for Rechargeable Battery: In-situ Recipe

2020 ◽  
Vol 170 ◽  
pp. 01018
Author(s):  
Nishigandh Pande ◽  
Adinath Jambhale ◽  
Dipika Jaspal ◽  
Jalinder Ambekar ◽  
Himanshu Patil
Keyword(s):  
Cost Effective ◽  
Rechargeable Battery ◽  
Discharge Process ◽  
X Ray Diffraction ◽  
One Pot ◽  
X Ray ◽  
In Situ Method ◽  
Mechanism Of Interaction ◽  
Uv Visible

The synthesis of cost-effective and safe polymeric nanocomposite materials has been a subject of interest and study for material science researchers. Poly (N-Methyl Aniline) –Li nanocomposite has been synthesized by a one-pot in-situ method and has been explored as an electrolyte in the battery. Poly (N-Methyl Aniline)-Li nanocomposite prepared, has been characterized by UV-visible, FTIR, FE-SEM, X-ray diffraction techniques. A mechanism of interaction of lithiumion with nitrogen at the imine site has been proposed. The charge-discharge process of poly (N-Methyl Aniline) –Li nanocomposite, when used in the battery, has been discussed.

Preparation and Crystal Structure of the Potentially Tridentate Substituted Phenoxyacetic Acid (2-Benzoyl-5-methoxyphenoxy)acetic Acid and Its Complex Adduct With Sodium

1995 ◽  
Vol 48 (4) ◽  
pp. 869 ◽  
Author(s):  
G Smith ◽  
EJ Oreilly ◽  
SA See ◽  
KA Byriel ◽  
CHL Kennard
Keyword(s):  
Crystal Structure ◽  
Acetic Acid ◽  
Carboxy Group ◽  
Intramolecular Hydrogen Bonding ◽  
Ligand Molecule ◽  
Phenoxyacetic Acid ◽  
X Ray Diffraction ◽  
X Ray ◽  
Intramolecular Hydrogen ◽  
Hydrogen Bonded

The ring-substituted phenoxyacetic acid (2-benzoyl-5-methoxyphenoxy)acetic acid (HL) (3) and its complex adduct dimer (4) with sodium, [Na2(L)2(HL)2].2HL, have been synthesized and their structures determined by X-ray diffraction. The acid (3) does not have the usual cyclic hydrogen-bonded dimer association, but instead has three-centre intramolecular hydrogen bonding between the carboxyl proton and both the ether and keto oxygens [O---O, 2.602(3), 2.711(3) Ǻ respectively]. Each sodium in the centrosymmetric complex dimer (4) is seven-coordinate [Na-O, 2.313(5)-2.612(5) Ǻ], involving the 'inner' three oxygens of both a protonated and an ionic ligand molecule. In addition, one of these carboxyl oxygens forms a bridge to the inversion-related sodium, while the uncoordinated carboxyl oxygen is hydrogen-bonded to a protonated carboxy group [O---O, 2.464(8) Ǻ]. The molecules of the lattice acid have only one hydrogen-bonded association with the second uncoordinated carboxy group in the dimer [O---O, 2.513(7) Ǻ].

The Na—O bond in sodium fenamate

2019 ◽  
Vol 75 (5) ◽  
pp. 766-774 ◽  
Author(s):  
Marta S. Krawczyk ◽  
Irena Majerz
Keyword(s):  
Noncovalent Interaction ◽  
Sodium Cation ◽  
Water Molecules ◽  
X Ray Diffraction ◽  
Surrounding Water ◽  
Polymeric Structure ◽  
One Dimensional ◽  
X Ray ◽  
The One ◽  
Intramolecular Hydrogen

The one-dimensional polymeric structure of sodium diaquafenamate–water (1/1) was studied by X-ray diffraction. The sodium cation is coordinated to one oxygen atom of the carboxylate group and to four water oxygen atoms. To characterize the Na—O bonds, the quantum theory of atoms in molecules (QTAIM) and noncovalent interaction (NCI) approaches have been used. Both methods confirmed that the Na—O bonds are very weak, comparable with the weak N—H...O intramolecular hydrogen bond. The polymeric structure is stabilized by the interaction of the sodium cation with the surrounding water molecules.

scholarly journals Hemi-Synthesis of Chiral Imine, Benzimidazole and Benzodiazepines from Essential Oil of Ammodaucus leucotrichus subsp. leucotrichus

Molecules ◽  
2019 ◽  
Vol 24 (5) ◽  
pp. 975 ◽  
Author(s):  
Farid Chebrouk ◽  
Khodir Madani ◽  
Brahim Cherfaoui ◽  
Leila Boukenna ◽  
Mónica Válega ◽  
...  
Keyword(s):  
Essential Oil ◽  
Hplc Analysis ◽  
Reaction Medium ◽  
2D Nmr ◽  
Chiral Hplc ◽  
X Ray Diffraction ◽  
X Ray ◽  
Reaction Proceeds ◽  
Derivatives Of

The hemi-synthesis of chiral imine, benzimidazole and benzodiazepine structures is reported by the condensation of (S)-(−)-perillaldehyde, the major phytochemical of Ammodaucus leucotrichus subsp. leucotrichus essential oil, with different amine derivatives of 2,3-diaminomaleonitrile, o-phenylenediamine and 3-[(2-aminoaryl)amino]dimedone. The reaction proceeds in situ at ambient temperature without prior isolation of the natural (S)-(−)-perillaldehyde. Final products precipitate in the ethanolic reaction medium. 2D NMR and single-crystal X-ray diffraction studies were used to unequivocally characterize the structures in solution and in the solid state, respectively. Chiral HPLC analysis confirms the formation of unique enantiomers and diastereomeric mixtures.

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