N-(Carboxymethyl)-N-[2-(2,6-diisopropylphenyl)amino]-2-oxoethylglycine and analogues: Synthesis and characterization

1982 ◽  
Vol 35 (11) ◽  
pp. 2371 ◽  
Author(s):  
MP Best ◽  
RH McKeown ◽  
O Wong
Keyword(s):  
General Procedure ◽  
Synthesis And Characterization ◽  
Reaction Conditions ◽  
One Pot ◽  
Specific Reaction ◽  
The Stability

N-(Carboxymethyl)-N-[2-(2,6-diisopropylphenyl)amino]-2-oxoethylglycine (DIS-IDA)* (2a) and two analogues have been successfully synthesized. The synthesis involved a modified one-pot reaction with specific reaction conditions to maximize yields. A general procedure for the isolation of the products has been set out and the stability of compounds (2) is briefly discussed. Characterization is reported with a view for use with 99mTc as radiopharmaceuticals.

Synthesis and Characterization of Substituted μ-oxo-bis[tetra-phenylporphyrinatoiron] Compounds

2015 ◽  
Vol 748 ◽  
pp. 183-186
Author(s):  
Zhi Cheng Sun ◽  
Shu Ying Chen ◽  
Zhi Peng Guo ◽  
Mei Juan Cao ◽  
Lu Hai Li
Keyword(s):  
Infrared Spectra ◽  
Elemental Analysis ◽  
Aromatic Aldehydes ◽  
Synthesis And Characterization ◽  
Visible Spectroscopy ◽  
Reaction Conditions ◽  
One Pot ◽  
Optimum Reaction ◽  
Novel Method

A novel one-pot method for the synthesis of substituted μ-oxo-bis [tetraphenyl porphyrinatoiron] compounds ([TRPPFe]2O) from pyrrole and aromatic aldehydes was proposed and investigated in this paper. Four kinds of [TRPPFe]2O were designed and synthesized by one-pot reaction and characterized by elemental analysis, infrared spectra and ultraviolet-visible spectroscopy. Moreover, the [TRPPFe]2O yields of 18.7~22.4% could be obtained with this novel method under the optimum reaction conditions.

Novel Magnetically Hollowsphere Zn-Doped Magnetite for the Efficient Photo-Reduction of Cr(VI)

2020 ◽  
Vol 9 (1) ◽  
Author(s):  
Sang Nguyen Xuan ◽  
Phuong Nguyen Thi Hong ◽  
Tung Vo Hoang
Keyword(s):  
Photocatalytic Activity ◽  
Hexavalent Chromium ◽  
Catalytic Mechanism ◽  
High Photocatalytic Activity ◽  
Reaction Conditions ◽  
One Pot ◽  
Morphology And Structure ◽  
Initial Ph ◽  
The Stability ◽  
Magnetic Recyclable

Uniform and magnetic recyclable hollowsphere Zn doped Fe3O4 were successfully synthesized via simple one-pot solvothermal route. Morphology and structure of as-obtained products was characterized by XRD, SEM, HRTEM methods. The Zn-doped Fe3O4 hollowsphere exhibited high photocatalytic activity for degradation of hexavalent chromium under visible light irradiation. The effects of reaction conditions such as initial pH, photocatalyst dosage and hexavalent chromium contratentation were also studied systematically. The stability of the catalysts and and possible catalytic mechanism was also proposed. The results indicate that Zn doped Fe3O4 can be promising catalyst for photo-reduction of hexavalent chromium.

First evidence of formation of stable DBU Zn-phthalocyanine complexes: synthesis and characterization

2005 ◽  
Vol 09 (07) ◽  
pp. 519-527 ◽  
Author(s):  
Roberta Del Sole ◽  
Agnese De Luca ◽  
Giuseppe Mele ◽  
Giuseppe Vasapollo
Keyword(s):  
Thermal Analysis ◽  
Axial Ligand ◽  
Synthesis And Characterization ◽  
One Pot ◽  
Strong Base ◽  
Pyridine Complex ◽  
The Stability ◽  
First Time ◽  
Complex Thermal Analysis

Novel Zn (II) phthalocyanine and naphthalocyanine DBU complexes have been prepared in a one-pot synthesis reacting phthalonitrile precursors with an excess of DBU (1,8-diazabicyclo[5.4.0]undec-7-ene). For the first time, it has been well evidenced that DBU played the role of coordinating axial ligand together with the well known role of strong base. Also, DBU complexes showed better solubility in organic solvents due to the coordination of the bulky axial DBU ligand, compared to the Zn (II) phthalocyanines and naphthalocyanines without coordinated DBU. The coordinating properties of DBU toward ZnPcs (DBU free) complexes have also been investigated along with the ZnPc (pyridine) complex. Thermal analysis results reflecting the stability of the synthesized complexes under air are also presented.

Solid State Analysis and Theoretical Explorations on Polymorphic and Hydrate Forms of p-Hydroxybenzaldehyde Isonicotinichydrazone: Effect of Additives on Polymorphic Crystallization

2018 ◽  
Author(s):  
Lincy Tom ◽  
Victoria A. Smolenski ◽  
Jerry P. Jasinski ◽  
M.R. Prathapachandra Kurup
Keyword(s):  
Hirshfeld Surface ◽  
Framework Analysis ◽  
Reaction Conditions ◽  
Space Groups ◽  
Effect Of Additives ◽  
Ft Ir ◽  
Packing Arrangement ◽  
The Stability ◽  
Ir And Raman ◽  
Isonicotinic Hydrazide

The reaction of p-hydroxybenzaldehyde with an equimolar amount of isonicotinic hydrazide afforded two polymorphic and hydrate forms of p-hydroxybenzaldehyde isonicotinichydrazone (HBIH) by varying the experimental reaction conditions. The compounds are fully characterized by means of single crystal and powder diffraction methods, vibrational spectroscopy (FT-IR and Raman), thermal and elemental analysis. The compound crystallizes in three different forms in two different space groups, P21/c (form PA and PB) and Pbca (PC). The Hirshfeld surface analysis shows the differences in the relative contributions of intermolecular interactions to the total Hirshfeld surface area for the HBIH molecules. The calculated pairwise interaction energies (104-116 kJ/mol) can be related to the stability of the crystals. Energy framework analysis identifies the interaction hierarchy and their topology. The geometry and conformation of the three forms are essentially similar which differ only by packing arrangement.

Solid State Analysis and Theoretical Explorations on Polymorphic and Hydrate Forms of p-Hydroxybenzaldehyde Isonicotinichydrazone: Effect of Additives on Polymorphic Crystallization

2018 ◽  
Author(s):  
Lincy Tom ◽  
Victoria A. Smolenski ◽  
Jerry P. Jasinski ◽  
M.R. Prathapachandra Kurup
Keyword(s):  
Hirshfeld Surface ◽  
Framework Analysis ◽  
Reaction Conditions ◽  
Space Groups ◽  
Effect Of Additives ◽  
Ft Ir ◽  
Packing Arrangement ◽  
The Stability ◽  
Ir And Raman ◽  
Isonicotinic Hydrazide

The reaction of p-hydroxybenzaldehyde with an equimolar amount of isonicotinic hydrazide afforded two polymorphic and hydrate forms of p-hydroxybenzaldehyde isonicotinichydrazone (HBIH) by varying the experimental reaction conditions. The compounds are fully characterized by means of single crystal and powder diffraction methods, vibrational spectroscopy (FT-IR and Raman), thermal and elemental analysis. The compound crystallizes in three different forms in two different space groups, P21/c (form PA and PB) and Pbca (PC). The Hirshfeld surface analysis shows the differences in the relative contributions of intermolecular interactions to the total Hirshfeld surface area for the HBIH molecules. The calculated pairwise interaction energies (104-116 kJ/mol) can be related to the stability of the crystals. Energy framework analysis identifies the interaction hierarchy and their topology. The geometry and conformation of the three forms are essentially similar which differ only by packing arrangement.

A Facile One-pot Synthesis of Substituted Quinolines via Cascade Friedlander Reaction from Isoxazoles with Ammonium Formate-Pd/C and Ketones

2020 ◽  
Vol 17 (3) ◽  
pp. 211-215
Author(s):  
Da Chen ◽  
Xuan Wang ◽  
Runnan Wang ◽  
Yao Zhan ◽  
Xiaohan Peng ◽  
...  
Keyword(s):  
Hydrogen Transfer ◽  
Ammonium Formate ◽  
Aromatic Ketone ◽  
Reaction Conditions ◽  
One Pot ◽  
Diverse Range ◽  
Strong Base ◽  
Aromatic Ketones ◽  
Substituted Quinolines ◽  
New Strategy

The Friedlander reaction is the most commonly used method to synthesis substituted quinolines, the essential intermediates in the medicine industry. A facile one-pot approach for synthesizing substituted quinolines by the reaction of isoxazoles, ammonium formate-Pd/C, concentrated sulfuric acid, methanol and ketones using Friedlander reaction conditions is reported. Procedures for the synthesis of quinoline derivatives were optimized, and the yield was up to 90.4%. The yield of aromatic ketones bearing electron-withdrawing groups was better than the ones with electron-donating substituents. The structures of eight substituted quinolines were characterized by MS, IR, H-NMR and 13CNMR, which were in agreement with the expected structures. The mechanism for the conversion was proposed, which involved the Pd/C catalytic hydrogen transfer reduction of unsaturated five-membered ring of isoxazole to produce ortho-amino aromatic ketones. Then the nucleophilic addition of with carbonyl of the ketones generated Schiff base in situ, which underwent an intermolecular aldol reaction followed by the elimination of H2O to give production of substituted quinolines. This new strategy can be readily applied for the construction of quinolines utilizing a diverse range of ketones and avoids the post-reaction separation of the o-amino aromatic ketone compounds. The conventionally used o-amino aromatic ketone compounds in Friedlander reaction to prepare substituted quinoline are laborious to synthesize and are apt to self-polymerize. While oxazole adopted in this work can be prepared at ease by the condensation of benzoacetonitrile and nitrobenzene derivatives under the catalysis of a strong base. Moreover, the key features of this protocol are readily available starting materials, excellent functional group tolerance, mild reaction conditions, operational simplicity, and feasibility for scaling up.

Novel One-pot Synthesis of Pyranocarbazole Derivatives via an Isocyanide-based Three-component Reaction

2020 ◽  
Vol 17 ◽  
Author(s):  
Visarapu Malathi ◽  
Pedavenkatagari Narayana Reddy ◽  
Pannala Padmaja
Keyword(s):  
Efficient Method ◽  
Atom Economy ◽  
Reaction Conditions ◽  
One Pot ◽  
Catalyst Free ◽  
One Pot Synthesis ◽  
Three Component Reaction ◽  
High Yields

Abstract:: An efficient method has been developed for the synthesis of new pyrano[3,2-c] and pyrano[3,2-a]carbazole de-rivatives via a three component reaction of 4-hydroxycarbazole or 2-hydroxycarbazole, isocyanides, and dialkylacetylenedi-carboxylates. Noteworthy features of this protocol include mild reaction conditions, catalyst-free, high atom-economy and high yields.

One-pot Synthesis of Pyrazolone Sulfones by Iodine-catalyzed Sulfenylation of Pyrazolones with Aryl Sulfonyl Hydrazides Followed by Oxidation in Water

2018 ◽  
Vol 15 (3) ◽  
pp. 380-387
Author(s):  
Xia Zhao ◽  
Xiaoyu Lu ◽  
Lipeng Zhang ◽  
Tianjiao Li ◽  
Kui Lu
Keyword(s):  
Double Bond ◽  
Efficient Method ◽  
Room Temperature ◽  
Sulfonyl Chloride ◽  
Antibacterial Activities ◽  
Oxidation Reactions ◽  
Reaction Conditions ◽  
One Pot ◽  
X Ray ◽  
Amide Form

Aim and Objective: Pyrazolone sulfones have been reported to exhibit herbicidal and antibacterial activities. In spite of their good bioactivities, only a few methods have been developed to prepare pyrazolone sulfones. However, the substrate scope of these methods is limited. Moreover, the direct sulfonylation of pyrazolone by aryl sulfonyl chloride failed to give pyrazolone sulfones. Thus, developing a more efficient method to synthesize pyrazolone sulfones is very important. Materials and Method: Pyrazolone, aryl sulphonyl hydrazide, iodine, p-toluenesulphonic acid and water were mixed in a sealed tube, which was heated to 100°C for 12 hours. The mixture was cooled to 0°C and m-CPBA was added in batches. The mixture was allowed to stir for 30 min at room temperature. The crude product was purified by silica gel column chromatography to afford sulfuryl pyrazolone. Results: In all cases, the sulfenylation products were formed smoothly under the optimized reaction conditions, and were then oxidized to the corresponding sulfones in good yields by 3-chloroperoxybenzoic acid (m-CPBA) in water. Single crystal X-ray analysis of pyrazolone sulfone 4aa showed that the major tautomer of pyrazolone sulfones was the amide form instead of the enol form observed for pyrazolone thioethers. Moreover, the C=N double bond isomerized to form an α,β-unsaturated C=C double bond. Conclusion: An efficient method to synthesize pyrazolone thioethers by iodine-catalyzed sulfenylation of pyrazolones with aryl sulfonyl hydrazides in water was developed. Moreover, this method was employed to synthesize pyrazolone sulfones in one-pot by subsequent sulfenylation and oxidation reactions.

Synthesis of Pyrrolo[1,2-a][1,6]- and [1,8]naphthyridines by Alkyne-Carbonyl Metathesis

Synthesis ◽  
2020 ◽  
Author(s):  
Peter Ehlers ◽  
Peter Langer ◽  
Marian Blanco Ponce ◽  
Silvio Parpart ◽  
Alexander Villinger ◽  
...  
Keyword(s):  
Heterocyclic Compounds ◽  
Metathesis Reaction ◽  
Synthetic Methodology ◽  
Facile Synthesis ◽  
Reaction Conditions ◽  
One Pot ◽  
Metal Free ◽  
Modular Synthesis

AbstractA concise and modular synthesis of pyrrolo[1,2-a][1,6]- and [1,8]naphthyridines by a one-pot two-step reaction consisting of electrophilic acylation followed by an alkyne-carbonyl-metathesis reaction as the final cyclization step is reported. This developed synthetic methodology allows the facile synthesis of these heterocyclic core structures in mainly high overall yields under metal-free conditions. Reaction conditions are carefully optimized and display a novel supplement to access these tricyclic heterocyclic compounds.

scholarly journals Integration of Stable Ionic Liquid-Based Nanofluids into Polymer Membranes. Part I: Membrane Synthesis and Characterization

Nanomaterials ◽  
2021 ◽  
Vol 11 (3) ◽  
pp. 607
Author(s):  
Carolina Hermida-Merino ◽  
Fernando Pardo ◽  
Gabriel Zarca ◽  
João M. M. Araújo ◽  
Ane Urtiaga ◽  
...  
Keyword(s):  
Polymer Membranes ◽  
Small Addition ◽  
Polymeric Membranes ◽  
Synthesis And Characterization ◽  
Complete Disappearance ◽  
Optical Profilometry ◽  
Scanning Calorimetry ◽  
Exfoliated Graphene ◽  
The Stability ◽  
Scanning Electron

In this work, polymeric membranes functionalized with ionic liquids (ILs) and exfoliated graphene nanoplatelets (xGnP) were developed and characterized. These membranes based on graphene ionanofluids (IoNFs) are promising materials for gas separation. The stability of the selected IoNFs in the polymer membranes was determined by thermogravimetric analysis (TGA). The morphology of membranes was characterized using scanning electron microscope (SEM) and interferometric optical profilometry (WLOP). SEM results evidence that upon the small addition of xGnP into the IL-dominated environment, the interaction between IL and xGnP facilitates the migration of xGnP to the surface, while suppressing the interaction between IL and Pebax®1657. Fourier transform infrared spectroscopy (FTIR) was also used to determine the polymer–IoNF interactions and the distribution of the IL in the polymer matrix. Finally, the thermodynamic properties and phase transitions (polymer–IoNF) of these functionalized membranes were studied using differential scanning calorimetry (DSC). This analysis showed a gradual decrease in the melting point of the polyamide (PA6) blocks with a decrease in the corresponding melting enthalpy and a complete disappearance of the crystallinity of the polyether (PEO) phase with increasing IL content. This evidences the high compatibility and good mixing of the polymer and the IoNF.

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