scholarly journals Catalyzed Reaction of Cellulose and Lignin with Methyltrimethoxysilane—FT-IR, 13C NMR and 29Si NMR Studies

Materials ◽  
2019 ◽  
Vol 12 (12) ◽  
pp. 2006 ◽  
Author(s):  
Joanna Siuda ◽  
Waldemar Perdoch ◽  
Bartłomiej Mazela ◽  
Magdalena Zborowska
Keyword(s):  
Acetic Acid ◽  
Ir Spectra ◽  
Atomic Absorption ◽  
13C Nmr ◽  
Atomic Absorption Spectroscopy ◽  
Reaction Mechanisms ◽  
29Si Nmr ◽  
Nmr Studies ◽  
Nmr Techniques ◽  
Ft Ir

It can be found that reaction mechanisms and interactions between wood and organosilicone compounds have not been sufficiently explored. The aim of the study was to determine bonds formed between either cellulose or lignin and methyltrimethoxysilane (MTMOS) during a catalytic silanization reaction. Silanization was performed in the presence of two catalysts of a diverse mechanism of functionalization: aluminum acetylacetonate (Al(acac)3) and acetic acid (AcOH). For this purpose, FT-IR, 13C and 29Si NMR techniques were used. Cellulose silanization efficiency without a catalyst was unlikely. Lignin undergoes a silanization reaction with alkoxysilanes much easier than cellulose. The results showed new bonds between biopolymers and the silanising agent. The new bonds were confirmed by signals at the FT-IR spectra, e.g., 770 cm−1 and 1270 cm−1 (Si–CH3), and at the NMR signal coming from the T1, T2 and T3 structures. Efficiency of reaction was confirmed by atomic absorption spectroscopy (AAS) analysis.

New Ferrocene-Integrated Multifunctional Guanidine Surfactants: Synthesis, Spectroscopic Elucidation, DNA Interaction Studies, and DFT Calculations

2021 ◽  
Author(s):  
Sameen Nawaz ◽  
Faiza Asghar ◽  
Jahangeer Patujo ◽  
Saira Fatima ◽  
Babar Murtaza ◽  
...  
Keyword(s):  
Dft Calculations ◽  
Atomic Absorption ◽  
Absorption Spectroscopy ◽  
13C Nmr ◽  
Atomic Absorption Spectroscopy ◽  
Analytical Methods ◽  
Dna Interaction ◽  
Interaction Studies ◽  
Ft Ir

Three new ferrocene-substituted aliphatic guanidines were successfully synthesized and well characterized by means of several analytical methods such as: FT-IR, 1H & 13C-NMR, Raman, atomic absorption spectroscopy (AAS), and elemental...

scholarly journals Quinazolin-4(3H)-ones and 5,6-Dihydropyrimidin-4(3H)-ones from β-Aminoamides and Orthoesters

Molecules ◽  
2018 ◽  
Vol 23 (11) ◽  
pp. 2925 ◽  
Author(s):  
Joshua Gavin ◽  
Joel Annor-Gyamfi ◽  
Richard Bunce
Keyword(s):  
Acetic Acid ◽  
Melting Point ◽  
1H Nmr ◽  
13C Nmr ◽  
Pressure Tube ◽  
Absolute Ethanol ◽  
Basic Nitrogen ◽  
One Step ◽  
Ft Ir

Quinazolin-4(3H)-ones have been prepared in one step from 2-aminobenzamides and orthoesters in the presence of acetic acid. Simple 2-aminobenzamides were easily converted to the heterocycles by refluxing in absolute ethanol with 1.5 equivalents of the orthoester and 2 equivalents of acetic acid for 12–24 h. Ring-substituted and hindered 2-aminobenzamides as well as cases incorporating an additional basic nitrogen required pressure tube conditions with 3 equivalents each of the orthoester and acetic acid in ethanol at 110 °C for 12–72 h. The reaction was tolerant towards functionality on the benzamide and a range of structures was accessible. Workup involved removal of the solvent under vacuum and either recrystallization from ethanol or trituration with ether-pentane. Several 5,6-dihydropyrimidin-4(3H)-ones were also prepared from 3-amino-2,2-dimethylpropionamide. All products were characterized by melting point, FT-IR, 1H-NMR, 13C-NMR, and HRMS.

scholarly journals Synthesis and Characterization of Some Novel Oxazine, Thiazine and Pyrazol Derivatives

2016 ◽  
Vol 13 (2) ◽  
pp. 244-252
Author(s):  
Baghdad Science Journal
Keyword(s):  
Acetic Acid ◽  
Ir Spectra ◽  
Glacial Acetic Acid ◽  
Basic Medium ◽  
Synthesis And Characterization ◽  
Pyrazole Derivatives ◽  
Phenyl Hydrazine ◽  
H Nmr ◽  
Ft Ir

In this paper, some chalcone derivatives (C1, C2) were synthesized based on the reaction of equal amount of substituted acetophenone and substituted banzaldehyde in basic medium. Oxazine and thiazine derivatives were prepared from the reaction of chalcones (C1-C2) with urea and thiourea respectively in a basic medium. Pyrazole derivatives were prepared based on the reaction of chalcones with hydrazine mono hydrate or phenyl hydrazine in the presence of glacial acetic acid as a catalyst. The new synthesized compounds were identified using various physical techniques like1 H-NMR and FT-IR spectra.

scholarly journals Synthesis, Characterization and In-Silico Analysis of New 2-Pyrazolines

2021 ◽  
Vol 13 (1) ◽  
pp. 183-194
Author(s):  
T. Saroja ◽  
R. M. Ezhilarasi ◽  
V. Selvamani ◽  
S. Mahalakshmi
Keyword(s):  
Acetic Acid ◽  
13C Nmr ◽  
Heterocyclic Compounds ◽  
Mass Spectra ◽  
Acid Hydrazide ◽  
In Silico Analysis ◽  
Pharmacological Activities ◽  
Cyclocondensation Reaction ◽  
Ft Ir ◽  
Silico Analysis

Heterocyclic compounds such as pyrazolines, pyrimidines, oxazole and isoxazole exhibit different pharmacological activities. The current study involves synthesis of new 2-pyrazolines. The synthesis involves the cyclocondensation reaction of substituted chalcones with (4-fluorophenylthio)acetic acid hydrazide (FTAH) under reflux. The chalcones (C1-C7 / 1a-1g) were synthesized from the reaction of substituted acetophenone with substituted benzaldehyde and FTAH was prepared from 4-fluro thiophenol. New 2-pyrazolines were obtained in good yields (60-70 %). All the compounds were characterized by FT-IR, 1H, 13C NMR and mass spectra. PASS analysis was carried out for the 2-pyrazolines synthesized (P1-P7 / 3a-3g).

scholarly journals Synthesis of Novel N-Acylhydrazones and Their C-N/N-N Bond Conformational Characterization by NMR Spectroscopy

Molecules ◽  
2021 ◽  
Vol 26 (16) ◽  
pp. 4908
Author(s):  
Rubina Munir ◽  
Noman Javid ◽  
Muhammad Zia-ur-Rehman ◽  
Muhammad Zaheer ◽  
Rahila Huma ◽  
...  
Keyword(s):  
13C Nmr ◽  
Nmr Spectra ◽  
Room Temperature ◽  
Aromatic Aldehydes ◽  
Spectral Studies ◽  
13C Nmr Spectra ◽  
1H And 13C Nmr ◽  
Mass Spectral ◽  
Nmr Techniques ◽  
Ft Ir

In this article, a synthesis of N’-(benzylidene)-2-(6-methyl-1H-pyrazolo[3,4-b]quinolin-1-yl)acetohydrazides and their structural interpretation by NMR experiments is described in an attempt to explain the duplication of some peaks in their 1H- and 13C-NMR spectra. Twenty new 6-methyl-1H-pyrazolo[3,4-b]quinoline substituted N-acylhydrazones 6(a–t) were synthesized from 2-chloro-6-methylquinoline-3-carbaldehyde (1) in four steps. 2-Chloro-6-methylquinoline-3-carbaldehyde (1) afforded 6-methyl-1H-pyrazolo[3,4-b]quinoline (2), which upon N-alkylation yielded 2-(6-methyl-1H-pyrazolo[3,4-b]quinolin-1-yl)acetate (3). The hydrazinolysis of 3 followed by the condensation of resulting 2-(6-methyl-1H-pyrazolo[3,4-b]quinolin-1-yl)acetohydrazide (4) with aromatic aldehydes gave N-acylhydrazones 6(a–t). Structures of the synthesized compounds were established by readily available techniques such as FT-IR, NMR and mass spectral studies. The stereochemical behavior of 6(a–t) was studied in dimethyl sulfoxide-d6 solvent by means of 1H NMR and 13C NMR techniques at room temperature. NMR spectra revealed the presence of N’-(benzylidene)-2-(6-methyl-1H-pyrazolo[3,4-b]quinolin-1-yl)acetohydrazides as a mixture of two conformers, i.e., E(C=N)(N-N) synperiplanar and E(C=N)(N-N)antiperiplanar at room temperature in DMSO-d6. The ratio of both conformers was also calculated and E(C=N) (N-N) syn-periplanar conformer was established to be in higher percentage in equilibrium with the E(C=N) (N-N)anti-periplanar form.

scholarly journals Synthesis, characterization and Cytotoxicity Evaluation of New Compounds from Oxazol-5(4H)-Ones and 1,2,4-Triazin-6(5H)-Ones Classes

2019 ◽  
Vol 70 (11) ◽  
pp. 3769-3774
Author(s):  
Elena Valentina Rosca ◽  
Theodora Venera Apostol ◽  
Constantin Draghici ◽  
Octavian Tudorel Olaru ◽  
Laura Ileana Socea ◽  
...  
Keyword(s):  
Acetic Acid ◽  
Acetic Anhydride ◽  
Elemental Analysis ◽  
13C Nmr ◽  
Heterocyclic Compounds ◽  
Sodium Acetate ◽  
Artemia Salina ◽  
Ft Ir ◽  
New Compounds ◽  
Acetic Acids

This paper presents the synthesis of new heterocyclic compounds from oxazoles and triazinones classes. Some 2-(4-(4-X-phenylsulfonyl)benzamido)acetic acids were condensed with 4-iodobenzaldehyde in presence of acetic anhydride and sodium acetate, when the new corresponding unsaturated oxazol-5(4H)-one were obtained. Through the reaction of these oxazol-5(4H)-ones with phenylhydrazine, in presence of the acetic acid and sodium acetate, the new heterocyclic compounds from 1,2,4-triazin-6(5H)-ones class were obtained. The structures of synthesized compounds have been confirmed by spectral methods (FT-IR, 1H-NMR, 13C-NMR and MS) and elemental analysis. The cytotoxicity of the compounds was evaluated using the Daphnia magna and Artemia salina bioassays.

scholarly journals Synthesis, characterization and Cytotoxicity Evaluation of New Compounds from Oxazol-5(4H)-Ones and 1,2,4-Triazin-6(5H)-Ones Classes

2019 ◽  
Vol 70 (11) ◽  
pp. 3769-3774
Author(s):  
Elena Valentina Rosca ◽  
Theodora Venera Apostol ◽  
Constantin Draghici ◽  
Octavian Tudorel Olaru ◽  
Laura Ileana Socea ◽  
...  
Keyword(s):  
Acetic Acid ◽  
Acetic Anhydride ◽  
Elemental Analysis ◽  
13C Nmr ◽  
Heterocyclic Compounds ◽  
Sodium Acetate ◽  
Artemia Salina ◽  
Ft Ir ◽  
New Compounds ◽  
Acetic Acids

This paper presents the synthesis of new heterocyclic compounds from oxazoles and triazinones classes. Some 2-(4-(4-X-phenylsulfonyl)benzamido)acetic acids were condensed with 4-iodobenzaldehyde in presence of acetic anhydride and sodium acetate, when the new corresponding unsaturated oxazol-5(4H)-one were obtained. Through the reaction of these oxazol-5(4H)-ones with phenylhydrazine, in presence of the acetic acid and sodium acetate, the new heterocyclic compounds from 1,2,4-triazin-6(5H)-ones class were obtained. The structures of synthesized compounds have been confirmed by spectral methods (FT-IR, 1H-NMR, 13C-NMR and MS) and elemental analysis. The cytotoxicity of the compounds was evaluated using the Daphnia magna and Artemia salina bioassays.

scholarly journals Caracterización geoquímica de las partículas atmosféricas sedimentables recolectadas en estaciones de servicio de la ciudad de Cumaná, noreste de Venezuela

2018 ◽  
Vol 5 (1) ◽  
pp. 57-62
Author(s):  
Adriana Gamboa ◽  
Carlos Álvarez
Keyword(s):  
Acetic Acid ◽  
Atomic Absorption ◽  
Atomic Absorption Spectroscopy ◽  
Soxhlet Extraction ◽  
Residual Fraction ◽  
Emission Sources ◽  
Organic Fraction ◽  
Bioavailable Fraction ◽  
Service Stations ◽  
Petrol Pump

Las estaciones de servicio (E/S) pueden aportar contaminantes al aire, suelo y los cuerpos de agua. Con la finalidad de analizar la concentración biodisponible (bio) y residual (res) de; y la fracción orgánica (FO) en partículas atmosféricas sedimentables recolectadas E/S de la ciudad, se tomaron muestras en tres estaciones, considerando tres lugares de muestreo (entrada, surtidor y salida), durante tres semanas. Para la determinación de metales biodisponibles, las muestras (<50 mallas) se agitaron a temperatura ambiente con CH3COOH durante 5 horas. El residuo se trató a 80 ºC con HNO3-HCl (3:1), para obtener la fracción residual. La concentración de metales se determinó por espectroscopia de absorción atómica y la FOE por extracción Soxhlet. La acumulación de las especies químicas resultó mayor en el área del surtidor, lo que implica que es el lugar de muestreo idóneo para analizar el impacto de las E/S como fuentes contaminantes. Existieron diferencias significativas (p<0,05) en las medianas de Fe(bio), Pb(res) y FOE en función del lugar de la toma y la estación, lo que permite inferir posibles diferencias en las fuentes de emisión y las condiciones de acumulación de estos. La correlación positiva entre Fe(bio) con Ni(bio) y FOE; y de Fe(res) con Pb(res), indica la asociación de las especies de acuerdo a las fuentes de emisión.     ABSTRACT Services stations can provide contaminants into the air, soils, and waterbodies. In order to analyze Fe, Pb, Cd, Ni residual and bioavailable content, and organic fraction (OF) associated to atmospheric settled particles, samples were taken in three service stations of Cumaná city (northeastern Venezuela), considering three sampling sites (1) entry; (2) petrol pump, and exit, for three weeks. The metals bioavailable fraction analyses consisted in stir the samples at lab temperature with acetic acid for 5 hours. The residue was treated at 80 ° C with HNO3-HCl (3:1), to obtain the residual fraction. The concentration of metals was determined by atomic absorption spectroscopy and organic fraction by Soxhlet extraction. At the petrol pump, more metals were accumulated, which implies that it is an ideal place to carry out impact studies of service stations as fixed sources of pollutants. There were significant differences (p <0,05) in the medians of Fe (bio), Pb (res) and OF according to the sampling sites, and the services stations: Which allows to infer possible differences in emission sources and accumulationconditions. The positive correlation between Fe (bio) with Ni (bio) and OF; and of Fe (res) with Pb (res), indicates the association of the species according to the emission sources.  

scholarly journals Pengaruh Variasi Jenis Pelarut pada Rendemen Sintesis Senyawa Kompleks Bis-Asetilasetonatodiaquonikel(II)

2015 ◽  
Vol 18 (1) ◽  
pp. 29-33
Author(s):  
Novia Mintari ◽  
Suhartana Suhartana ◽  
Sriatun Sriatun
Keyword(s):  
Fourier Transform ◽  
Atomic Absorption ◽  
Absorption Spectroscopy ◽  
Atomic Absorption Spectroscopy ◽  
Infra Red ◽  
Ft Ir

Sintesis Senyawa Kompleks Bis-Asetilasetonatodiaquonikel(II)  telah dilakukan. Penelitian ini bertujuan untuk untuk mensintesis senyawa kompleks bis-asetilasetonatodiaquonikel(II) ([Ni(acac)2(H2O)2]) dengan menggunakan pelarut metanol, etanol dan aseton serta membandingkan pengaruh pelarut yang digunakan terhadap hasil sintesis senyawa kompleks. Senyawa kompleks [Ni(acac)2(H2O)2] dibuat dengan memodifikasi metode Pawlikowski dengan perbandingan mol ion pusat dengan ligan adalah 1:3. Karakterisasi senyawa kompleks dilakukan menggunakan Fourier Transform-Infra Red (FT-IR), Atomic Absorption Spectroscopy (AAS), dan Spektrofotometer UV-Vis. Hasil FTIR menunjukkan adanya gugus O pada asetil aseton yang terkoordinasi pada ion pusat Ni2+ membentuk kompleks [Ni(acac)2(H2O)2]. Spektra UV-Vis menghasilkan serapan maksimum untuk kompleks [Ni(acac)2(H2O)2] dalam pelarut metanol pada panjang gelombang 294,5 nm, dengan energi transisi sebesar 406,72 KJmol-1, dan rendemen 19,26%. Kompleks [Ni(acac)2(H2O)2] dalam pelarut etanol memiliki panjang gelombang maksimum pada 294,5 nm, dengan energi transisi sebesar 406,72 KJmol-1, dan rendemen 18,69%. Sedangkan kompleks [Ni(acac)2(H2O)2] dalam pelarut aseton mempunyai panjang gelombang maksimum pada 293 nm, dengan energi transisi sebesar 408,80 KJmol-1, dan rendemen 16,99%.

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