scholarly journals Synthesis, crystal structure and antioxidant evaluation of N-(4-formylpiperazine-1-carbonothioyl)benzamide

2020 ◽  
Vol 11 (2) ◽  
pp. 156-159 ◽  
Author(s):  
Hamza Milad Abosadiya
Keyword(s):  
13C Nmr Spectroscopy ◽  
Carbonyl Groups ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
1H And 13C Nmr ◽  
Triclinic Crystal System ◽  
X Ray ◽  
Dpph Method ◽  
Antioxidant Evaluation ◽  
Ft Ir

New benzoylthiourea derivative, N-(4-formylpiperazine-1-carbonothioyl)benzamide was prepared by the reaction of benzoylisothiocyanate with 1-piperazinecarboxaldehyde in acetone as solvent. The compound was characterized by FT-IR and multinuclear 1H and 13C NMR spectroscopy techniques. The benzoylthiourea molecule was obtained in crystalline form by recrystallization in DMSO. Single crystal X-ray diffraction study indicates that compound crystallized in triclinic crystal system and crystal data for C13H15N3O2S, space group P-1 (no. 2), a = 7.3016(9) Å, b = 7.7380(9) Å, c = 12.9815(16) Å, α = 103.581(4)°, β = 102.153(4)°, γ = 102.409(4)°, V = 669.46(14) Å3, Z = 2, T = 296(2) K, μ(MoKα) = 0.243 mm-1, Dcalc = 1.376 g/cm3, 31184 reflections measured (6.72° ≤ 2Θ ≤ 53.46°), 2822 unique (Rint = 0.0582) which were used in all calculations. The final R1 was 0.0501 (>2σ(I)) and wR2 was 0.1493 (all data). Intramolecular N-H···O hydrogen bond is stabilized the trans geometry of the thiono and the carbonyl groups. The heterocyclic piperazine ring makes a dihedral angle of 48.50(15)° with the benzene ring. Antioxidant test by DPPH method showed that compound exhibits good antioxidant activity of about 75%.

Synthesis, Characterization, and Catalytic Activity of a Series of Aluminium–Amidate Complexes

2015 ◽  
Vol 68 (3) ◽  
pp. 357 ◽  
Author(s):  
Kevin P. Yeagle ◽  
Darryl Hester ◽  
Nicholas A. Piro ◽  
William G. Dougherty ◽  
W. Scott Kassel ◽  
...  
Keyword(s):  
Catalytic Activity ◽  
Nmr Spectroscopy ◽  
Diffraction Analysis ◽  
13C Nmr ◽  
13C Nmr Spectroscopy ◽  
X Ray Diffraction ◽  
Metathesis Reaction ◽  
Chloride Complexes ◽  
1H And 13C Nmr ◽  
X Ray

The aluminium complexes {[κ2-N,O-(t-BuNCOPh)]AlMe2}2 (2), [κ2-N,O-(t-BuNCOPh)]2AlMe (3), and [κ2-N,O-(t-BuNCOPh)]3Al (4) were prepared through the protonolysis reaction between trimethylaluminium and one, two, or three equivalents, respectively, of N-tert-butylbenzamide. Complex 2 was also prepared via a salt metathesis reaction between K(t-BuNCOPh) and dimethylaluminium chloride. Complexes 2–4 were characterized using 1H and 13C NMR spectroscopy. Single-crystal X-ray diffraction analysis of the complexes corroborated ligand : metal stoichiometries and revealed that all the amidate ligands coordinate to the aluminium ion in a κ2 fashion. The Al–amidate complexes 2–4 were viable catalyst precursors for the Meerwein–Ponndorf–Verley–Oppenauer reduction–oxidation manifold, successfully interconverting several classes of carbonyl and alcohol substrates.

scholarly journals Synthesis and Characterization of Ammonium Acesulfamate

2014 ◽  
Vol 69 (6) ◽  
pp. 737-741 ◽  
Author(s):  
Gustavo A. Echeverría ◽  
Oscar E. Piro ◽  
Beatriz S. Parajón-Costa ◽  
Enrique J. Baran
Keyword(s):  
Molecular Structure ◽  
Ammonium Carbonate ◽  
Crystal And Molecular Structure ◽  
13C Nmr Spectroscopy ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
1H And 13C Nmr ◽  
X Ray

Ammonium acesulfamate, (NH4)C4H4NO4S, was prepared by the reaction of acesulfamic acid and ammonium carbonate in aqueous solution, and characterized by elemental analysis and 1H and 13C NMR spectroscopy. Its crystal and molecular structure was determined by single-crystal X-ray diffraction methods. The substance crystallizes in the orthorhombic space group Pnma with Z = 4 molecules per unit cell. The NH4+ ion generates medium to strong hydrogen bonds with the carbonylic oxygen, the iminic nitrogen and the sulfonyl oxygen atoms of the acesulfamate anion. The FTIR spectrum of the compound was also recorded and is briefly discussed.

Ageing mechanisms of the papers with zeolite and PCC fillers

2021 ◽  
Vol 0 (0) ◽  
Author(s):  
Merve Engin ◽  
Nural Yılgör ◽  
Celil Atik
Keyword(s):  
Attenuated Total Reflectance ◽  
Accelerated Ageing ◽  
Carbonyl Groups ◽  
X Ray Diffraction ◽  
Precipitated Calcium Carbonate ◽  
Total Reflectance ◽  
X Ray ◽  
Ft Ir ◽  
Diagnosis Approach

Abstract This work has been conducted to investigate the effect of accelerated ageing on the filler-free (control) handsheets and the ones having Precipitated Calcium Carbonate (PCC) and Zeolite (Clinoptilolite) fillers. The diagnosis approach of this work has been based on the use of the techniques of attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR) and X-ray diffraction (XRD). The FT-IR technique has allowed identifying the changes in cellulose components of handsheets. Likewise, the XRD technique has provided to diagnose the changes in crystallinity of the handsheets and fillers. The results found out that PCC and Zeolite fillers could be easily added to the structure of the paper network by changing various experimental variables. The loss of C−O functional groups and the formation of carbonyl groups in handsheets has been analysed by accelerated ageing. The spectroscopy results confirmed that usage of zeolite filler has a retarding and structurally improving effect on the glycosidic linkages. Recent findings have been provided new insights into the role of the synergistic effect of the combination of PCC and zeolite fillers in the decelerating of certain ageing mechanism.

scholarly journals Synthesis, Crystal Structure and Bioactivity of Phenazine-1-carboxylic Acylhydrazone Derivatives

Molecules ◽  
2021 ◽  
Vol 26 (17) ◽  
pp. 5320
Author(s):  
Shouting Wu ◽  
Xi Liang ◽  
Fang Luo ◽  
Hua Liu ◽  
Lingyi Shen ◽  
...  
Keyword(s):  
Carboxylic Acid ◽  
Condensation Reaction ◽  
Acid Hydrazide ◽  
13C Nmr Spectroscopy ◽  
X Ray Diffraction ◽  
1H And 13C Nmr ◽  
X Ray ◽  
Thiazolyl Blue Tetrazolium Bromide ◽  
Thiazolyl Blue Tetrazolium

A phenazine-1-carboxylic acid intermediate was synthesized from the reaction of aniline and 2-bromo-3-nitro-benzoic acid. It was then esterified and reacted with hydrazine hydrate to afford phenazine-1-carboxylic hydrazine. Finally, 10 new hydrazone compounds 3a–3j were obtained by the condensation reaction of phenazine-1-carboxylic acid hydrazide and the respective aldehyde-containing compound. The structures were characterized by 1H and 13C NMR spectroscopy, MS and single crystal X-ray diffraction. The antitumor activity of the target compounds in vitro (HeLa and A549) was determined by thiazolyl blue tetrazolium bromide. The results showed that compound (E)-N′-(2-hydroxy-4-(2-(piperidine-1-yl) ethoxy) benzyl) phenazine-1-carbonyl hydrazide 3d exhibited good cytotoxic activity.

scholarly journals Synthesis, structural and conformational study of selected N-substituted phthalimides

2005 ◽  
Vol 3 (4) ◽  
pp. 683-704 ◽  
Author(s):  
Isabel Iriepa ◽  
F. Javier Villasante ◽  
Enrique Gálvez ◽  
Antonio Herrera ◽  
Angel Sánchez ◽  
...  
Keyword(s):  
Double Resonance ◽  
13C Nmr Spectroscopy ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
1H And 13C Nmr ◽  
Conformational Studies ◽  
One Dimensional ◽  
X Ray ◽  
Nmr Techniques ◽  
New Compounds

AbstractThis paper synthesizes N-substituted phthalimides derived from nitrogen heterocycles as potential 5-HT4 ligands by using the Mitsunobu reaction. Conformational studies of some of the new compounds have been conducted using 1H and 13C-NMR spectroscopy. Proton and carbon resonances were achieved through the application of one-dimensional selective NOE, two-dimensional NMR techniques-homonuclear COSY-45, NOESY and heteronuclear 1H-13C HMQC correlated spectroscopy- and double resonance experiments. The crystal structure of compound 1 was determined by X-ray diffraction.

An Improved Synthesis of 3,6-Dihydro-as-indacene

Synthesis ◽  
2020 ◽  
Author(s):  
Marcelo Preite ◽  
Elies Molins ◽  
Ivonne Chávez ◽  
Mungalimane K. Amshumali ◽  
Cesar Morales-Verdejo ◽  
...  
Keyword(s):  
Ammonium Hydroxide ◽  
13C Nmr Spectroscopy ◽  
X Ray Diffraction ◽  
1H And 13C Nmr ◽  
Intramolecular Cycloaddition ◽  
X Ray ◽  
Full Characterization ◽  
Mannich Condensation ◽  
Acidic Conditions

AbstractThis contribution describes an updated synthetic route to 3,6-dihydro-as-indacene along with full characterization of all inter­mediates. The title compound is prepared by Mannich condensation of 2-methylfuran with formaldehyde and dimethylamine hydrochloride, quaternization of the resulting amine with methyl iodide, and conversion into the ammonium hydroxide salt by treatment with silver oxide in water. Subsequent Hoffmann elimination and [6,6]-cycloaddition through pyrolysis produces a furanocyclophane, which after photooxidation, intramolecular cycloaddition, and dehydration with sodium carbonate affords 2,3,6,7-tetrahydro-1,8-dione-as-indacene. Reduction of this diketone gives a mixture of alcohols, which after dehydration under slightly basic or acidic conditions produces 3,6-dihydro-as-indacene. The structure is confirmed by X-ray diffraction, and all intermediates are characterized by means of 1H and 13C NMR spectroscopy.

scholarly journals A molecular inclusion complex of atenolol with 2-hydroxypropyl-β-cyclodextrin: The production and characterization thereof

2007 ◽  
Vol 72 (8-9) ◽  
pp. 737-746 ◽  
Author(s):  
Vesna Nikolic ◽  
Ljubisa Nikolic ◽  
Mihajlo Stankovic ◽  
Agnes Kapor ◽  
Mirjana Popsavin ◽  
...  
Keyword(s):  
Inclusion Complex ◽  
1H Nmr ◽  
13C Nmr ◽  
Chemical Shifts ◽  
13C Nmr Spectroscopy ◽  
X Ray Diffraction ◽  
X Ray ◽  
Molecular Inclusion ◽  
Ft Ir ◽  
Diffraction Patterns

The molecular inclusion complex of atenolol with 2-hydroxypropyl-?-cyclodextrin was synthesized using the coprecipitation method. The complex obtained was characterized by FT-IR, 1H-NMR, 13C-NMR spectroscopy, as well as by DSC and X-ray diffraction analysis. The DSC analysis confirmed the existence of the complex with the endothermic atenolol melting peak at about 155?C disappearing. The X-ray diffraction patterns of the complex and 2-hydroxypropyl-?-cyclodextrin were very similar, thus confirming the complete inclusion of the atenolol molecule within the cavity of the 2-hydroxypropyl-?-cyclodextrin. The peaks originating from atenolol were completely absent in the diffractogram of the complex. 1H-NMR and 13C-NMR spectra showed certain changes in the chemical shifts of protons and C atoms from atenolol and 2-hydroxypropyl-?-cyclodextrin, indicating that a complex had been formed and also which protons participated in the hydrogen bonds which formed the complex. The atenolol solubility in water was improved (254 mg complex cm-3, i.e., 37.5 mg atenolol cm-3), and in pH 3 HCl solution (251 mg complex cm-3, i.e., 37 mg atenolol cm-3) when compared to pure atenolol, and even when compared to the atenolol complex with ?-cyclodextrin. The increased solubility ensures greater bioavailability of the active component and, due to the low solubility, significantly corrects for the lack of the basic active substance and, simultaneously, increases its overall therapeutic effect, combined with reduced side effects. .

scholarly journals Anticancer Diiron Vinyliminium Complexes: A Structure–Activity Relationship Study

Pharmaceutics ◽  
2021 ◽  
Vol 13 (8) ◽  
pp. 1158
Author(s):  
Simona Braccini ◽  
Giorgia Rizzi ◽  
Lorenzo Biancalana ◽  
Alessandro Pratesi ◽  
Stefano Zacchini ◽  
...  
Keyword(s):  
Cell Line ◽  
Cancer Cell ◽  
Thioredoxin Reductase ◽  
Cancer Cell Line ◽  
13C Nmr Spectroscopy ◽  
X Ray Diffraction ◽  
1H And 13C Nmr ◽  
X Ray ◽  
Screening Study ◽  
The Stability

A series of 16 novel diiron complexes of general formula [Fe2Cp2(CO)(μ-CO){μ-η1:η3-C(R′)C(R″)CN(R)(Y)}]CF3SO3 (2–7), bearing different substituents on the bridging vinyliminium ligand, was synthesized in 69–95% yields from the reactions of diiron μ-aminocarbyne precursors with various alkynes. The products were characterized by elemental analysis, IR, 1H and 13C NMR spectroscopy; moreover the X-ray structures of 2c (R = Y = CH2Ph, R′ = R″ = Me) and 3a (R = CH2CH=CH2, Y = R′ = Me, R″ = H) were ascertained by single-crystal X-ray diffraction studies. NMR and UV–Vis methods were used to assess the D2O solubility, the stability in aqueous solution at 37 °C and the octanol–water partition coefficients of the complexes. A screening study evidenced a potent cytotoxicity of 2–7 against the A2780 cancer cell line, with a remarkable selectivity compared to the nontumoral Balb/3T3 cell line; complex 4c (R = Cy, Y = R′ = R″ = Me) revealed as the most performant of the series. The antiproliferative activity of a selection of complexes was also assessed on the cisplatin-resistant A2780cisR cancer cell line, and these complexes were capable of inducing a significant ROS production. Moreover, ESI-MS experiments indicated the absence of interaction of selected complexes with cytochrome c and the potentiality to inhibit the thioredoxin reductase enzyme (TrxR).

Solid state and solution stereochemistry of crown ethers and models. ortho-Dimethoxydiphenyl ether and related dibenzo-15-crown-5 and tetrabenzo-30-crown-10 ethers as studied by X-ray crystallography and 1H and 13C NMR spectroscopy

1994 ◽  
Vol 72 (5) ◽  
pp. 1218-1224 ◽  
Author(s):  
G. W. Buchanan ◽  
A. Rodrigue ◽  
K. Bourque ◽  
A. C. Chiverton ◽  
I. R. Castleden ◽  
...  
Keyword(s):  
Solid Phase ◽  
Direct Methods ◽  
13C Nmr Spectroscopy ◽  
Structural Features ◽  
X Ray Diffraction ◽  
1H And 13C Nmr ◽  
Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
C Nmr

Solid phase 45.3 MHz 13C NMR spectra of ortho-dimethoxydiphenyl ether, 1, dibenzo[b,e]-15-crown-5- ether, 2, and tetrabenzo[b,e,q,t]-30-crown-10 ether, 3, have been obtained. Chemical shift trends are discussed in terms of the asymmetric units and structural features available from X-ray crystallographic data. Comparison with solution 13C spectra are made. The crystal structures of 1 and 3 were determined by X-ray diffraction at room temperature. 1 crystallizes in space group P21/a with a = 13.366(1), b = 8.230(1), c = 12.303(1) Å, β = 116.63(1)°, Z = 4. 3 crystallizes in space group P21/c with a = 7.903(1), b = 26.337(2), c = 7.852(1) Å, β = 97.28(1)°, Z = 2. The structures were solved by direct methods and refined by full-matrix least squares to residuals of 0.055 using 1727 reflections for 1 and of 0.042 using 2590 reflections for 3.

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