scholarly journals Synthesis of 1-aryl-1-phenylpropenes using an alkylation-rearrangement-methylation-isomerization one-pot reaction sequence

2011 ◽  
Vol 9 (5) ◽  
pp. 904-909 ◽  
Author(s):  
Nenad Maraš ◽  
Franc Perdih ◽  
Marijan Kočevar
Keyword(s):  
Claisen Rearrangement ◽  
Structural Features ◽  
X Ray Diffraction ◽  
Reaction Sequence ◽  
One Pot ◽  
Double Bond Migration ◽  
X Ray ◽  
Crystalline Product ◽  
Tetramethylammonium Chloride ◽  
The One

Abstract(Z/E)-1-(2-Methoxyaryl)-1-phenylpropenes have been prepared in good yields by heating a mixture of a phenolic substrate, cinnamyl chloride, tetramethylammonium chloride and K2CO3 in polyethyleneglycol at 180°C. The one-pot synthesis proceeds through four discrete reaction steps: alkylation of the phenol with cinnamyl chloride, Claisen rearrangement, O-methylation and double-bond migration. The configuration of one crystalline product was determined using a single-crystal X-ray diffraction analysis. The thermodynamic and structural features of the products were evaluated using computational chemistry techniques.

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 Water-Soluble O-, S- and Se-Functionalized Cyclic Acetyl-triaza-phosphines. Synthesis, Characterization and Application in Catalytic Azide-alkyne Cycloaddition

Molecules ◽  
2020 ◽  
Vol 25 (22) ◽  
pp. 5479
Author(s):  
Abdallah Mahmoud ◽  
Piotr Smoleński ◽  
M. Guedes da Silva ◽  
Armando Pombeiro
Keyword(s):  
Cycloaddition Reaction ◽  
Structural Features ◽  
Water Soluble ◽  
31P Nmr Spectroscopy ◽  
The Novel ◽  
X Ray Diffraction ◽  
One Pot ◽  
Hirshfeld Surfaces ◽  
The One ◽  
High Yields

The 3,7-diacetyl-1,3,7-triaza-5-phosphabicyclo[3.3.1]nonane (DAPTA) derivatives, viz. the already reported 3,7-diacetyl-1,3,7-triaza-5-phosphabicyclo[3.3.1]nonane 5-oxide (DAPTA=O, 1), the novel 3,7-diacetyl-1,3,7-triaza-5-phosphabicyclo[3.3.1]nonane-5-sulfide (DAPTA=S, 2), and 3,7-diacetyl-1,3,7-triaza-5-phosphabicyclo[3.3.1]nonane-5-selenide (DAPTA=Se, 3), have been synthesized under mild conditions. They are soluble in water and most common organic solvents and have been characterized using 1H and 31P NMR spectroscopy and, for 2 and 3, also by single crystal X-ray diffraction. The effect of O, S, or Se at the phosphorus atom on the structural features of the compounds has been investigated, also through the analyses of Hirshfeld surfaces. The presence of 1–3 enhances the activity of copper for the catalytic azide-alkyne cycloaddition reaction in an aqueous medium. The combination of cheaply available copper (II) acetate and compound 1 has been used as a catalyst for the one-pot and 1,4-regioselective procedure to obtain 1,2,3-triazoles with high yields and according to ‘click rules’.

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 

Syntheses and molecular structures of some di(amidino)monosilanes

2021 ◽  
Vol 44 (1) ◽  
pp. 228-238
Author(s):  
Markus Bös ◽  
Marcus Herbig ◽  
Uwe Böhme ◽  
Edwin Kroke
Keyword(s):  
Raman Spectroscopy ◽  
Single Crystal ◽  
High Field ◽  
Structural Features ◽  
Molecular Structures ◽  
X Ray Diffraction ◽  
One Pot ◽  
X Ray ◽  
Field Shift ◽  
Nmr Signals

Abstract The syntheses of three different amidinosilanes of the type Me2Si[N=C(Ph)R]2 with R = pyrrolidino, morpholino, and diethylamino and one derivative with the composition R2Si[N=C(Ph)R]2 with R = morpholino are reported. These compounds were prepared in one-pot syntheses including three consecutive steps. All products are analysed by single crystal X-ray diffraction, NMR, and Raman spectroscopy. The Si–N=C–N units of these compounds show characteristic structural features and cause a significant high field shift of the 29Si NMR signals.

scholarly journals One-Pot Hydrothermal Synthesis, Characterization, and Desulfurization Performance of ZnFe2O4/AC Composites

2018 ◽  
Vol 2018 ◽  
pp. 1-10 ◽  
Author(s):  
Hui-qiang Wang ◽  
Ming-hua Liu ◽  
Xin Luo ◽  
Yi-fan Liu ◽  
Fei-er Chen ◽  
...  
Keyword(s):  
Adsorption Capacity ◽  
Photoelectron Spectroscopy ◽  
Performance Test ◽  
X Ray Diffraction ◽  
One Pot ◽  
X Ray ◽  
Synthesis Conditions ◽  
Ft Ir ◽  
The One ◽  
Sulfur Adsorption

ZnFe2O4/AC composites were prepared by the one-pot hydrothermal method using the activated carbon (AC) as a carrier. The synthesis conditions were optimized by a single-factor experiment. The structural, textural, and surface properties of the adsorbent have been comprehensively characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier-transform infrared (FT-IR) spectroscopy, Brunauer–Emmett–Teller (BET) measurements, and X-ray photoelectron spectroscopy (XPS) analysis. The SO2 removal capacities of the composites were investigated via testing the adsorption capacity at the self-made desulfurization equipment. The results show that the adsorption capacity of ZnFe2O4/AC composites is much higher than that of the AC and ZnFe2O4 samples, respectively. The composite overcomes the disadvantages of the traditional sintering, showing a very high desulfurization performance. The breakthrough time was 147 min, and the sulfur adsorption capacity could reach 23.67% in the desulfurization performance test.

Purification and Functionalization of Diamond Nanopowders

2009 ◽  
Vol 1203 ◽  
Author(s):  
Jong-Kwan Lim ◽  
Jong-Beom Baek
Keyword(s):  
Chemical Modification ◽  
Polyphosphoric Acid ◽  
Wide Angle ◽  
X Ray Diffraction ◽  
Phosphorous Pentoxide ◽  
One Pot ◽  
X Ray ◽  
Diamond Nanopowder ◽  
The One ◽  
Diamond Nanopowders

AbstractPurification of diamond nanopowder (DNP) was conducted in a less-destructive mild polyphosphoric acid (PPA)/phosphorous pentoxide (P2O5). The wide-angle X-ray diffraction (XRD) showed that the intensity of the characteristic diamond d-spacing (111) at 2.07 Å from purified DNP (PDNP) was fairly increased compared to pristine DNP, indicating that significant amount of carbonaceous impurities were removed. Chemical modification of pristine DNP and PDNP with 4-ethylbenzoic acid was carried out to afford 4-ethylbenzoyl-functionalized DNP (EBA-g-DNP) and PDNP (EBA-g-PDNP). The morphologies of EBA-g-DNP and EBA-g-PDNP from scanning electron microscopy (SEM) were further affirmed the feasibility of chemical modification. The results suggested that the reaction condition was indeed viable for the one-pot purification and functionalization of DNP. The resultant functionalized DNP could be useful for nanoscale additives. Hence, EBA-g-DNP and EBA-g-PDNP was brominated by using N-bromosuccinimide (NBS). The resultant N-brominated DNP and PDNP could be used as initiator for the atom transfer radical polymerization (ATRP) to introduce many polymers onto the surface of functionalized DNP and PDNP.

scholarly journals Three Multi-Components Reaction: Synthesis and X-Ray Single-Crystal of Hydroacridinone-Based Hydrazino-S-Triazine Derivative as a New Class of Urease Inhibitor

Crystals ◽  
2019 ◽  
Vol 10 (1) ◽  
pp. 14 ◽  
Author(s):  
Assem Barakat ◽  
Saied M. Soliman ◽  
Ayman El-Faham ◽  
M. Ali ◽  
Abdullah Mohammed Al-Majid ◽  
...  
Keyword(s):  
Structural Features ◽  
Acetohydroxamic Acid ◽  
Orthorhombic Crystal System ◽  
Orthorhombic Crystal ◽  
One Pot ◽  
X Ray ◽  
New Class ◽  
Hirshfeld Surfaces ◽  
The One

The one-pot fashion of three multi-component reaction provides the desired hydroacridinone-based hydrazino-s-triazine scaffold 4. Compound 4 was crystallized in an orthorhombic crystal system and Pbca space group with a = 11.6271(2) Å, b = 18.2018(4) Å, c = 32.4721(6) Å, and α = β = γ = 90° with one formula unit per asymmetric unit and eight molecules per unit cell. Additionally, structural features, Hirshfeld surfaces, and DFT studies were also investigated. Its packing in the crystal is controlled by H…H (63.4%), O…H (12.7%), Cl…H (7.2%), N…H (4.7%), and C…H (10.2%) contacts, where the O…H and Cl…H contacts were found the strongest. In vitro urease inhibition evaluation showed that the hydroacridinone-based hydrazino-s-triazine is more active (IC50 = 17.9 ± 0.47 µM) than the standard acetohydroxamic acid (IC50 = 20.3 ± 0.43 µM).

The Construction of the Heterostructural Bi2O3/g-C3N4 Composites with an Enhanced Photocatalytic Activity

NANO ◽  
2018 ◽  
Vol 13 (06) ◽  
pp. 1850063 ◽  
Author(s):  
Jinhua Zhang ◽  
Huiyue Qian ◽  
Wencheng Liu ◽  
Hao Chen ◽  
Yang Qu ◽  
...  
Keyword(s):  
Photocatalytic Activity ◽  
Photoelectron Spectroscopy ◽  
Photogenerated Electron ◽  
X Ray Diffraction ◽  
One Pot ◽  
X Ray ◽  
Air Atmosphere ◽  
Transmission Electron ◽  
Ft Ir ◽  
The One

A heterostructural composite composed of g-C3N4 and Bi2O3 was achieved by the one-pot and thermal-induced polycondensation method using melamine and Bi(NO[Formula: see text] as precursor at 550[Formula: see text]C under air atmosphere. The crystalline phase, components and morphologies of the as-prepared composites were investigated by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM). Besides, the photocatalytic activity of composites was evaluated by degrading RhB aqueous solution at room temperature under visible light irradiation. Compared with bulk g-C3N4, the photocatalytic efficiency of the 0.5% Bi2O3/g-C3N4 (Bi–CN) was increased by up to four times. The introduction of Bi2O3 enhances not only the light absorption ability, but also the separation of photogenerated electron–hole pairs.

scholarly journals Solvent-free synthesis of 1-amidoalkyl-2-naphthol and 3-amino-1-phenyl-1H benzo[f]chromene-2-carbonitrile derivatives by Fe3O4@enamine-B(OSO3H)2 as an efficient and novel heterogeneous magnetic nanostructure catalyst

2020 ◽  
Vol 22 (2) ◽  
pp. 9-19 ◽  
Author(s):  
Fangping Li ◽  
Jun Zhang ◽  
Longjiang Wang ◽  
Weijian Liu ◽  
Qahtan A. Yousif
Keyword(s):  
Reaction Times ◽  
Catalytic Amount ◽  
X Ray Diffraction ◽  
One Pot ◽  
X Ray ◽  
Magnetic Nanostructure ◽  
The One ◽  
High Yields ◽  
Green Procedure ◽  
Work Up

AbstractA green procedure for the one-pot three-component synthesis of 1-amidoalkyl-2-naphthol and 3-amino-1-phenyl-1H benzo[f]chromene-2-carbonitrile derivatives from the reaction of 2-naphtol, aldehydes, and malononitrile/acetamide in the presence of a catalytic amount of Fe3O4@enamine-B(OSO3H)2 as an efficient and novel heterogeneous magnetic nanostructure catalyst is described. The catalyst was characterized using Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), vibrating sample magnetometry (VSM), energy dispersive X-ray spectroscopy (EDX), and X-ray diffraction (XRD). These strategies possess some merits such as simple work-up method, easy preparation of the catalyst, short reaction times, good-to-high yields, and non-use of hazardous solvents during all steps of the reactions. Moreover, due to the magnetic nature of the catalyst, it was readily recovered by magnetic decantation and can be recycled at least six runs with no considerable decrease in catalytic activity.

scholarly journals PREPARATION SOME ACID-ACTIVATED MONTMORILLONITES FROM CU CHI CLAY AND USING AS CATALYST IN ONE-POT CONVERSION OF BENZALDEHYDE INTO BENZONITRILE

2011 ◽  
Vol 14 (4) ◽  
pp. 43-53
Author(s):  
Dung Duc Pham ◽  
Dat Thanh Vu ◽  
Thach Ngoc Le
Keyword(s):  
Chemical Composition ◽  
Cation Exchange Capacity ◽  
Chemical Properties ◽  
Exchange Capacity ◽  
Solid Catalyst ◽  
X Ray Diffraction ◽  
One Pot ◽  
X Ray ◽  
Physical Chemical ◽  
The One

Montmorillonite is a "green" solid catalyst and support used in many organic reactions. In this paper, we have prepared some acid-activated montmorillonites from Cu Chi clay. Then, we determinated physical-chemical properties such as specific surface area, cation exchange capacity, X-ray diffraction, chemical composition and acidity of these samples. Finally, we chose the best from these montmorillonites and used as catalyst in the one-pot conversion of benzaldehyde into benzonitrile under solvent-free and microwave irradiation.

Sign in / Sign up

Export Citation Format

Share Document