Diversity-Oriented Synthesis of Novel Trihalomethyl-Containing Spirochromeno[3,4-a](thia)pyrrolizidines and Spirochromeno-[3,4-a]indolizidines by One-Pot, Three-Component [3+2]-Cyclo­addition Reaction

AbstractRegio- and stereoselective methods for the synthesis of 6′-trifluoro(trichloro)methyl substituted spiro[acenaphthylene-1,11′-chromeno[3,4-a](thia)pyrrolizidin]-2-ones and spiro[acenaphthylene-1,12′-chromeno[3,4-a]indolizidin]-2-ones have been developed based on the three-component reaction of 3-nitro-2-trifluoro(trichloro)methyl-2H-chromenes with azomethine ylides generated in situ from acenaphthenequinone and cyclic α-amino acids. The cycloaddition proceeds under mild conditions in ethanol or DMSO, and only endo-isomers of the products with cis-arrangement of nitro and trifluoromethyl groups are formed. The relative configuration of cycloadducts is reliably confirmed by X-ray diffraction analysis and by 2D NOESY spectroscopy.

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

E3S Web of Conferences ◽

10.1051/e3sconf/202017001018 ◽

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.

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A Convenient Synthesis of Fused Tetrahydroazocines from Acenaphthylene-1,2-dione, Proline, and Acetylenic Esters

Synlett ◽

10.1055/s-0036-1591855 ◽

2017 ◽

Vol 29 (05) ◽

pp. 635-639 ◽

Cited By ~ 6

Author(s):

Issa Yavari ◽

Leila Baoosi ◽

Mohammad Halvagar

Keyword(s):

Cycloaddition Reaction ◽

Azomethine Ylides ◽

Dipolar Cycloaddition ◽

X Ray Diffraction ◽

Acetylenic Esters ◽

X Ray ◽

Convenient Synthesis ◽

Boat Form ◽

Twist Boat

A synthesis of dialkyl (12E,14E)-7-oxo-10,11-dihydro-7H,9H-azocino[2,1-a]benzo[de]isoquinoline-13,14-dicarboxylates through a 1,3-dipolar cycloaddition reaction of azomethine ylides, generated in situ from proline and acenaphthylene-1,2-dione, with dialkyl acetylenedicarboxylates is described. According to the X-ray diffraction data, the tetrahydroazocine ring has a rigid twist-boat form with approximate local C2 symmetry.

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Design, Construction, and Characterization of a New Regioisomer and Diastereomer Material Based on the Spirooxindole Scaffold Incorporating a Sulphone Function

Symmetry ◽

10.3390/sym12081337 ◽

2020 ◽

Vol 12 (8) ◽

pp. 1337 ◽

Cited By ~ 1

Author(s):

Abdullah Mohammed Al-Majid ◽

Saied M. Soliman ◽

Matti Haukka ◽

M. Ali ◽

Mohammad Shahidul Islam ◽

...

Keyword(s):

Chemical Shifts ◽

Cycloaddition Reaction ◽

X Ray Diffraction ◽

One Pot ◽

Catalyst Synthesis ◽

X Ray ◽

Reactivity Descriptors ◽

Three Component Reaction ◽

Hirshfeld Analysis ◽

Donor Acceptor

The 1,3-dipolar cycloaddition reaction is one of the most rapid, and efficient protocols to access, and construct highly divergent heterocycle chiral auxiliaries. Free catalyst synthesis of spirooxindole scaffold incorporating sulphone moiety via one pot–three component reaction of 6-chloro-isatin, L-proline, and the phenylvinylsulphone as dienophile is presented. The new regioisomer and diastereomer was isolated by precipitation without the tedious purification step, and then characterized via NMR and single crystal X-ray diffraction analysis. Using Hirshfeld analysis, the analysis of molecular packing was performed. It depended mainly on strong O…H and N…H interactions, and weak H…H, C…H, and Cl…H interactions as well. DFT calculations were used to optimize the experimental X-ray structure, which was found well matched with the calculated one. Reactivity descriptors based on the energies of the highest occupied (HOMO) and lowest unoccupied (LUMO) molecular orbitals were calculated. Additionally, the donor–acceptor interactions which stabilized the system via σ–σ*, π→π*, n→σ* and n→π* electron delocalization processes were also computed using NBO calculations. The net interaction energies are 49.96, 235.38, 179.66 and 107.06 kJ/mol, respectively. Additionally, the calculated NMR chemical shifts correlated well with the experimental data (R2=0.99).

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One-pot multicomponent synthesis of furo[3,2-c]coumarins promoted by amino-functionalized Fe3O4@SiO2 nanoparticles

Zeitschrift für Naturforschung B ◽

10.1515/znb-2016-0041 ◽

2016 ◽

Vol 71 (8) ◽

pp. 849-856 ◽

Cited By ~ 10

Author(s):

Javad Safaei-Ghomi ◽

Hossein Shahbazi-Alavi ◽

Pouria Babaei

Keyword(s):

Sio2 Nanoparticles ◽

Environmentally Benign ◽

Biological Applications ◽

X Ray Diffraction ◽

Multicomponent Synthesis ◽

One Pot ◽

Diversity Oriented Synthesis ◽

X Ray ◽

Ft Ir ◽

Ft Ir Spectroscopy

AbstractAmino-functionalized Fe3O4@SiO2 nanoparticles (Fe3O4@SiO2–NH2 NPs) were prepared by treating Fe3O4@SiO2 NPs with (3-aminopropyl)-triethoxysilane. They have been characterized by powder X-ray diffraction, vibrating sample magnetometer, scanning electronic microscopy, energy dispersive X-ray, thermogravimetric analysis and FT-IR spectroscopy. A neat, atom-economical, environmentally benign one-pot multicomponent synthetic route for the synthesis of furo[3,2-c]coumarins in good yields has been devised using the Fe3O4@SiO2–NH2 NPs. The present methodology can be used for the design of libraries and diversity-oriented synthesis, and has potential for biological applications and drug discovery.

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

Molecules ◽

10.3390/molecules26237297 ◽

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.

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The Use of Advanced Analytical Techniques for Characterization of the Chemical, Physical, and Crystallographic Nature of a Surface

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100071107 ◽

1973 ◽

Vol 31 ◽

pp. 132-133 ◽

Cited By ~ 1

Author(s):

R. E. Herfert

Keyword(s):

Surface Characterization ◽

Analytical Techniques ◽

X Ray Diffraction ◽

Depth Of Penetration ◽

X Ray ◽

The Past ◽

Transmission Electron ◽

Scanning Electron

Studies of the nature of a surface, either metallic or nonmetallic, in the past, have been limited to the instrumentation available for these measurements. In the past, optical microscopy, replica transmission electron microscopy, electron or X-ray diffraction and optical or X-ray spectroscopy have provided the means of surface characterization. Actually, some of these techniques are not purely surface; the depth of penetration may be a few thousands of an inch. Within the last five years, instrumentation has been made available which now makes it practical for use to study the outer few 100A of layers and characterize it completely from a chemical, physical, and crystallographic standpoint. The scanning electron microscope (SEM) provides a means of viewing the surface of a material in situ to magnifications as high as 250,000X.

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