One-pot synthesis of the new Hydroxamic acid and its complexes with metals

2022 ◽  
Vol 19 ◽  
Author(s):  
Gulu Abbasova ◽  
Ajdar Medjidov
Keyword(s):  
Nmr Spectroscopy ◽  
Thermogravimetric Analysis ◽  
Hydroxamic Acid ◽  
Uv Spectroscopy ◽  
Molar Ratio ◽  
One Pot ◽  
Ethanol Medium ◽  
Physicochemical Methods ◽  
Colored Complexes ◽  
First Time

Abstract: A one-pot conversion of 2-hydroxy-1-naphthoic aldehyde to hydroxamic acid was described. An efficient photoorganocatalytic method of synthesis was developed. The obtained hydroxamic acid was identified by various physicochemical methods such as IR, UV- and NMR-spectroscopy. Solid colored complexes of copper (II) and iron (II), respectively, green and brown colours with the obtained hydroxamic acid were synthesized in ethanol medium for the first time. The molar ratio of ligand and metal in the complex was 2:1. Their structures were established using IR, UV- spectroscopy and thermogravimetric analysis.

scholarly journals A mesostructured hybrid CTA–silica carrier for curcumin delivery

2020 ◽  
Vol 96 (1) ◽  
pp. 236-246
Author(s):  
Marta Gallo ◽  
Fabio Giudice ◽  
Mauro Banchero ◽  
Silvia Ronchetti ◽  
Luigi Manna ◽  
...  
Keyword(s):  
Water Solubility ◽  
Uv Spectroscopy ◽  
Sol Gel ◽  
Topical Administration ◽  
Release Mechanism ◽  
Active Principle ◽  
One Pot ◽  
Drug Release Mechanism ◽  
Sol Gel Synthesis ◽  
First Time

Abstract Curcumin is a natural active principle with antioxidant, antibacterial and anti-inflammatory properties. Its use is limited by a low water solubility and fast degradation rate, which hinder its bioavailability. To overcome this problem, curcumin can be delivered through a carrier, which protects the drug molecule and enhances its pharmacological effects. The present work proposes a simple one-pot sol–gel synthesis to obtain a hybrid carrier for curcumin delivery. The hybrid consists of a mesostructured matrix of amorphous silica, which stabilizes the carrier, and hexadecyltrimethylammonium (CTA), a surfactant where curcumin is dissolved to increase its water solubility. The carrier was characterized in terms of morphology (FESEM), physicochemical properties (XRD, FTIR, UV spectroscopy) and release capability in pseudo-physiological solutions. Results show that curcumin molecules were entrapped, for the first time, in a silica-surfactant mesostructured hybrid carrier. The hybrid carrier successfully released curcumin in artificial sweat and in a phosphate buffer saline solution, so confirming its efficacy in increasing curcumin water solubility. The proposed drug release mechanism relies on the degradation of the carrier, which involves the concurrent release of silicon. This suggests strong potentialities for topical administration applications, since curcumin is effective against many dermal diseases while silicon is beneficial to the skin.

scholarly journals Tannins of Tamarind Seed Husk: Preparation, Structural Characterization, and Antioxidant Activities

2011 ◽  
Vol 6 (6) ◽  
pp. 1934578X1100600 ◽  
Author(s):  
Puksiri Sinchaiyakit ◽  
Yohji Ezure ◽  
Sarin Sriprang ◽  
Supakorn Pongbangpho ◽  
Nasapon Povichit ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Antioxidant Activities ◽  
Uv Spectroscopy ◽  
Degree Of Polymerization ◽  
Dpph Assay ◽  
One Pot ◽  
Acetone Water ◽  
Seed Husk ◽  
C Nmr ◽  
Ir And Uv Spectroscopy

The high content (about 39%) of polymeric tannins in tamarind ( Tamarindus indica L.) seed husk (TSH) was demonstrated, and an extract (crude TSE) with a high content (about 94%) of polymeric tannins was prepared from TSH with a one pot extraction using ethanol/water (3:2, v/v). The crude TSE was further purified with Sephadex LH20 to give one fraction (metTSE) eluted with methanol/water (3:2, v/v) and another (acTSE) eluted with acetone/water (3:2, v/v). The tannins of acTSE were established as polymeric proanthocyanidins (PA) by 13C NMR spectroscopy; this was further confirmed by IR and UV spectroscopy, n-BuOH/HCl and vanillin assays, and from HPLC pattern. The ratio of procyanidins to prodelphinidins was 2:3, and the average degree of polymerization of acTSE was 7. Galloylated flavan-3-ols were not detected in acTSE. The main ingredients of metTSE were confirmed to be polymeric PA by 13C NMR spectroscopy. The antioxidant activities using DPPH and ABTS assays were investigated. The IC50 values of acTSE were 4.2±0.2 (DPPH assay) and 6.2±0.3 μg/mL (ABTS assay).

scholarly journals Isolation and Study of Abies Bark Proanthocyanidins

2019 ◽  
pp. 604-613
Author(s):  
Vladimir A. Levdansky ◽  
Alexander A. Kondrasenko ◽  
Alexander V.; Levdansky ◽  
Maxim A. Lutoshkin
Keyword(s):  
Nmr Spectroscopy ◽  
Hydrochloric Acid ◽  
13C Nmr ◽  
Maximum Yield ◽  
13C Nmr Spectroscopy ◽  
Optimal Conditions ◽  
Ethanol Medium ◽  
First Time ◽  
Water Alcohol Solutions ◽  
Water Alcohol

The process of proanthocyanidins isolation from abies bark by water and water-alcohol solutions containing 5, 10, 15 and 20 % ethanol was studied for the first time. The optimal conditions providing the maximum yield of proanthocyanidins were determined experimentally. It was shown that the use of 15-20 % water-alcohol solutions allows to increase the yield of proanthocyanidins from 0.33 to 0.38 %. The composition of the obtained proanthocyanidins was studied by UV, IR, and 13C NMR spectroscopy. The obtained proanthocyanidins were transformed into colored anthocyanidins in ethanol medium in the presence of hydrochloric acid. The flavonoids cyanidin and delphinidin were isolated and identified. It was established that the obtained proanthocyanidins mainly consist of procyanidin and prodelphinidin. It was shown that proanthocyanidins obtained from abies bark, in contrast to the proanthocyanidins isolated from pine bark described in the literature, contain gallic acid residues, which is typical for proanthocyanidins isolated from various types of tea

The regulation of hydrophilicity and hydrophobicity of carbon dots via a one-pot approach

2015 ◽  
Vol 3 (29) ◽  
pp. 6013-6018 ◽  
Author(s):  
Quan-Xing Mao ◽  
Wen-Jing Wang ◽  
Xin Hai ◽  
Yang Shu ◽  
Xu-Wei Chen ◽  
...  
Keyword(s):  
Carbon Source ◽  
Carbon Dots ◽  
Hydrothermal Process ◽  
Molar Ratio ◽  
One Pot ◽  
Ethanol Medium ◽  
Hydrophilicity And Hydrophobicity

The hydrophilicity or hydrophobicity of carbon dots is regulated by varying the H3PO4/ethanol molar ratio, via a hydrothermal process with 1-butyl-3-methylimidazolium hexafluorophosphate as the carbon source in a H3PO4–ethanol medium.

Synthesis of Protein-Directed Orange/Red-Emitting Copper Nanoclusters via Hydroxylamine Hydrochloride Reduction Approach and Their Applications on Hg2+ Sensing

NANO ◽  
2016 ◽  
Vol 11 (10) ◽  
pp. 1650108 ◽  
Author(s):  
Jie Xu ◽  
Bingyan Han
Keyword(s):  
Ph Value ◽  
Hydroxylamine Hydrochloride ◽  
Reducing Agent ◽  
Molar Ratio ◽  
Synthesis Process ◽  
Copper Nanoclusters ◽  
One Pot ◽  
Synthesis Conditions ◽  
First Time ◽  
Selection Of

Herein, we report a facile one-pot method for the synthesis of orange/red-emitting fluorescent copper nanoclusters (Cu NCs), in which bovine serum albumin (BSA) served as the capping scaffold (Cu NCs@BSA) and hydroxylamine hydrochloride (NH2OH[Formula: see text][Formula: see text][Formula: see text]HCl) as the reducing agent. To the best of our knowledge, this is the first time to adopt this mild reductant to synthesize fluorescent Cu NCs. The as-prepared Cu NCs@BSA exhibits strong orange or red fluorescence at room temperature depending on the synthesis process, and the maximum excitation and emission peaks were at 355[Formula: see text]nm and 615[Formula: see text]nm, 395[Formula: see text]nm and 645[Formula: see text]nm, respectively. Synthesis conditions including the amounts of NH2OH[Formula: see text][Formula: see text][Formula: see text]HCl, the selection of reducing agent, the molar ratio of BSA/Cu(NO3)2, the pH value, the reaction temperature, the reaction time, and various kinds of Cu sources have been systematically studied. Importantly, these Cu NCs exhibit excellent stability for at least 2 months when stored at 4[Formula: see text]C in the dark, and they also show strong oxidation resistance toward H2O2. Moreover, the prepared Cu NCs have been successfully applied to sensitively and selectively sensing Hg[Formula: see text] without suffering any interference from other metal ions and anions.

Übergangsmetallkomplexe mit Schwefelliganden, XIII* Synthesen und Reaktionen der 1,2-Benzoldithiolatomolybdat-Komplexe [MO(C6H4S2)3]n- (n = 0, 1, 2) und des Hydrid-Komplexes [Mo(H)(C6H4S2)3]3- / Transition Metal Complexes with Sulfur Ligands, XIII* Syntheses and Reactions of the 1,2-Benzenedithiolato Molybdate Complexes [MO(C6H4S2)3]n- - (n = 0 , 1, 2 ) and the Hydride Complex [Mo(H)(C6H4S2)3]3-

1985 ◽  
Vol 40 (3) ◽  
pp. 380-388 ◽  
Author(s):  
Dieter Sellmann ◽  
Lothar Zapf
Keyword(s):  
Nmr Spectroscopy ◽  
Transition Metal Complexes ◽  
Metal Hydride ◽  
Complex Salt ◽  
Alkyl Halides ◽  
Molar Ratio ◽  
Substitution Reactions ◽  
Hydride Complex ◽  
H Nmr ◽  
First Time

Modes of formation as well as redox and substitution reactions of the 1,2-benzenedithiolate complexes [Mo(C6H4S2)3]n- (n = 0, 1, 2, (3)) are described. [MoCl4(THF)2] with neutral C6H4(SH)2 gives the Mo(VI) complex [Mo(C6H4S2)3]; with C6H4S22-, however, the Mo(IV) complex [Mo(C6H4S2)3]2- can be isolated as the PPh4+ or NR4+ salt; in the course of the synthesis of (NMe4)2[Mo(C6H4S2)3] in MeOH/THF, the complex salt trans-(NMe4)2[Mo(C6H4S2)2(OCH3)2] is also obtained. Directly and controlled by pH, [Mo(VI)(C6H4S2)3] can be reduced by NaOH/MeOH to afford [Mo(V)(C6H4S2)3]- or [Mo(IV)(C6H4S2)3]2-. [Mo(VI)(C6H4S2)3] and (NMe4)2[Mo(IV)(C6H4S2)3] symproportionate in MeOH to yield (NMe4)[Mo(V)(C6H4S2)3] , which was isolated for the first time. When butyllithium reacts with [Mo(VI)(C6H4S2)3] in the molar ratio of 1:1, 2 :1 or 3:1, one obtains the Mo(V), Mo(IV) dithiolates or an orange complex, respectively. The latter is extremely H2O - as well as O2-sensitive; it is identified by its reactions with H2O , ROH, O2 , alkyl halides and NO as well as by 1H NMR spectroscopy as a salt containing the [MO(H)(C6H4S2)3]3- anion. [Mo(H)(C6H4S2)3]3- is the first example of an exclusively sulfur coordinated metal hydride complex. With NO it reacts in several steps yielding first N2O and [Mo(IV)(C6H4S2)3]2-; subsequently the Mo(IV) complex is reductively nitrosylated by further NO yielding cis-[Mo(NO)2(C6H4S2)2]2-, which is isolated as NMe4+ salt.

An Expeditious One-Pot Three-Component Synthesis of 4-Aryl-3,4-dihydrobenzo[g] quinoline-2,5,10(1H)-triones under Green Conditions

2020 ◽  
Vol 23 (23) ◽  
pp. 2626-2634
Author(s):  
Saiedeh Kamalifar ◽  
Hamzeh Kiyani
Keyword(s):  
Reaction Medium ◽  
Meldrum's Acid ◽  
Meldrum’S Acid ◽  
One Pot ◽  
One Pot Synthesis ◽  
Substituted Benzaldehydes ◽  
High Yields ◽  
First Time ◽  
Green Conditions

: An efficient and facial one-pot synthesis of 4-aryl-3,4-dihydrobenzo[g]quinoline- 2,5,10(1H)-triones was developed for the first time. The process proceeded via the three-component cyclocondensation of 2-amino-1,4-naphthoquinone with Meldrum’s acid and substituted benzaldehydes under green conditions. The fused 3,4-dihydropyridin-2(1H)- one-ring naphthoquinones have been synthesized with good to high yields in refluxing ethanol as a green reaction medium. This protocol is simple and effective as well as does not involve the assistance of the catalyst, additive, or hazardous solvents.

scholarly journals (2S,3R,6R)-2-[(R)-1-Hydroxyallyl]-4,4-dimethoxy-6-methyltetrahydro-2H-pyran-3-ol

Molbank ◽  
10.3390/m1140 ◽  
2020 ◽  
Vol 2020 (2) ◽  
pp. M1140
Author(s):  
Jack Bennett ◽  
Paul Murphy
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Ir Spectroscopy ◽  
13C Nmr ◽  
Conjugate Addition ◽  
13C Nmr Spectroscopy ◽  
One Pot ◽  
1H And 13C Nmr ◽  
Esi Mass Spectrometry ◽  
The One

(2S,3R,6R)-2-[(R)-1-Hydroxyallyl]-4,4-dimethoxy-6-methyltetrahydro-2H-pyran-3-ol was isolated in 18% after treating the glucose derived (5R,6S,7R)-5,6,7-tris[(triethylsilyl)oxy]nona-1,8-dien-4-one with (1S)-(+)-10-camphorsulfonic acid (CSA). The one-pot formation of the title compound involved triethylsilyl (TES) removal, alkene isomerization, intramolecular conjugate addition and ketal formation. The compound was characterized by 1H and 13C NMR spectroscopy, ESI mass spectrometry and IR spectroscopy. NMR spectroscopy was used to establish the product structure, including the conformation of its tetrahydropyran ring.

Amino- and sulfo-bifunctionalized hyper-crosslinked organic nanotube frameworks as efficient catalysts for one-pot cascade reactions

2019 ◽  
Vol 43 (5) ◽  
pp. 2269-2273 ◽  
Author(s):  
Guojie Meng ◽  
Shengguang Gao ◽  
Ying Liu ◽  
Li Zhang ◽  
Chunmei Song ◽  
...  
Keyword(s):  
Cascade Reactions ◽  
One Pot ◽  
First Time

The synthesis of amino- and sulfo-bifunctionalized hyper-crosslinked organic nanotube frameworks for one-pot cascade reactions was reported for the first time.

scholarly journals Radical Dehalogenation and Purine Nucleoside Phosphorylase E. coli: How Does an Admixture of 2′,3′-Anhydroinosine Hinder 2-fluoro-cordycepin Synthesis

Biomolecules ◽  
2021 ◽  
Vol 11 (4) ◽  
pp. 539
Author(s):  
Alexey L. Kayushin ◽  
Julia A. Tokunova ◽  
Ilja V. Fateev ◽  
Alexandra O. Arnautova ◽  
Maria Ya. Berzina ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Chemical Synthesis ◽  
Purine Nucleoside Phosphorylase ◽  
Purine Nucleoside ◽  
Preparative Synthesis ◽  
Nucleoside Phosphorylase ◽  
E Coli ◽  
First Time

During the preparative synthesis of 2-fluorocordycepin from 2-fluoroadenosine and 3′-deoxyinosine catalyzed by E. coli purine nucleoside phosphorylase, a slowdown of the reaction and decrease of yield down to 5% were encountered. An unknown nucleoside was found in the reaction mixture and its structure was established. This nucleoside is formed from the admixture of 2′,3′-anhydroinosine, a byproduct in the preparation of 3-′deoxyinosine. Moreover, 2′,3′-anhydroinosine forms during radical dehalogenation of 9-(2′,5′-di-O-acetyl-3′-bromo- -3′-deoxyxylofuranosyl)hypoxanthine, a precursor of 3′-deoxyinosine in chemical synthesis. The products of 2′,3′-anhydroinosine hydrolysis inhibit the formation of 1-phospho-3-deoxyribose during the synthesis of 2-fluorocordycepin. The progress of 2′,3′-anhydroinosine hydrolysis was investigated. The reactions were performed in D2O instead of H2O; this allowed accumulating intermediate substances in sufficient quantities. Two intermediates were isolated and their structures were confirmed by mass and NMR spectroscopy. A mechanism of 2′,3′-anhydroinosine hydrolysis in D2O is fully determined for the first time.

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