Synthesis and vibrational study of a 1:1 stoichiometric complex of hydronium tetrafluoroborate and 1,4,7,10,13,16-hexaoxacyclooctadecane (18-crown-6)

1982 ◽  
Vol 60 (7) ◽  
pp. 853-861 ◽  
Author(s):  
Robert Chênevert ◽  
André Rodrigue ◽  
Marie Pigeon-Gosselin ◽  
Rodrigue Savoie

The macrocyclic ether 1,4,7,10,13,16-hexaoxaoctadecane (18-crown-6) has the remarkable property of being able to transfer the hydronium (H3O+) ion from an aqueous solution to an organic medium. This property has been used to synthetize a 1:1 stoichiometric complex of this ether with hydronium tetrafluoroborate. This complex is very stable (mp 145 °C) and dissolves readily, without decomposition, in solvents such as CHCl3. The presence of the H3O+ and BF4− ions in the complex has been confirmed by chemical analysis, and by 1H nmr, Raman, and ir spectroscopy. The vibrational spectra indicate that a conformational change of the crown ether takes place in the complex over the temperature range −50 °C to −100 °C. The symmetry of the crown ether, which appears to be relatively high at room temperature, is considerably reduced below the transition temperature.

e-Polymers ◽  
2012 ◽  
Vol 12 (1) ◽  
Author(s):  
Hong Zhang ◽  
Limin Zang ◽  
Jiahe Luo ◽  
Jinshan Guo

AbstractThe UV-initiated emulsion polymerization of methyl methacrylate (MMA) in the presence of FeCl3 was studied. The photopolymerization presented high efficiency even though using a small percentage of photoinitiator. The entire polymerization could be performed within 10 min and displayed a conversion higher than 90% at ambient temperature. The particle sizes could be tuned in the range of 20-90 nm. The effects of content of initiator and emulsifying agent upon the reaction conversion, distribution of molecular weight, diameter of particles and glass-transition temperature were examined. 1H-NMR technique was used to investigate the structural properties of PMMA.


2008 ◽  
Vol 5 (3) ◽  
pp. 461-466 ◽  
Author(s):  
Y. Rajendra Prasad ◽  
A. Lakshmana Rao ◽  
R. Rambabu

In an effort to develop antimicrobial agents, a series of chalcones were prepared by Claisen-Schmidt condensation of appropriate acetophenones with appropriate aromatic aldehydes in the presence of aqueous solution of potassium hydroxide and ethanol at room temperature. The synthesized compounds were characterized by means of their IR,1H-NMR spectral data and elemental analysis. All the compounds were tested for their antibacterial and antifungal activities by the cup plate method.


1999 ◽  
Vol 77 (11) ◽  
pp. 1911-1921 ◽  
Author(s):  
G W Buchanan ◽  
M Gerzain ◽  
C I Ratcliffe

2H NMR line shapes have been obtained as a function of temperature for partially deuteriated 15-crown-5·NaI, 15-crown-5·NaClO4 and 21-crown-7·KI. Sudden changes in the line shapes above 330 K correspond to phase transitions: DSC shows transitions at 338, 347 K for 15-crown-5·NaI, and 356, 374, 383 K for 15-crown-5·NaClO4. The 2H NMR line shapes for the room temperature (RT) phases show the onset of a motion of the macrocycles above 200K, which is rapid a little above room temperature. Through detailed analysis of the complicated line shapes it has been shown that the most consistent interpretation of the dynamics in these RT phases is a "merry-go-round" type of motion similar to that found for 18-crown-6 and 12-crown-4 complexes in which O-CH2-CH2 units exchange sites around the ring, simultaneously adjusting their conformation to fit the site. In the high-temperature phases of all three complexes all the ring atoms are dynamically equivalent. This can only happen through a combination of increased symmetry and disorder for which possible models have been devised.Key words: 2H NMR, crown ether complexes, dynamics, disorder.


2011 ◽  
Vol 8 (2) ◽  
pp. 541-546 ◽  
Author(s):  
S. Sridhar ◽  
S. C. Dinda ◽  
Y. Rajendra Prasad

A series of new chalcones(3a-g)were prepared by Claisen-Schmidt condensation of 3-acetyl-2,5-dimethylfuran with various substituted aromatic aldehydes in presence of aqueous solution of potassium hydroxide and ethanol at room temperature. The synthesized chalcones were characterized by means of their IR,1H NMRspectral data and elemental analyses. When these chalcones were evaluated for antimicrobial and anti-inflammatory activities, some of them were found to possess significant activity, when compared to standard drugs.


2016 ◽  
Vol 45 (3) ◽  
pp. 1000-1006 ◽  
Author(s):  
Qiong Ye ◽  
Hui-Ting Wang ◽  
Lin Zhou ◽  
Li-Hui Kong ◽  
Heng-Yun Ye ◽  
...  

(15-Crown-5)(BiCl3) and (15-crown-5)(SbCl3) are discovered to show phase transitions above room temperature, where the phase transition temperature relates to the metal center.


2021 ◽  
Author(s):  
SEDA KARAYÜNLÜ BOZBAS ◽  
Begüm Canan Yıldız Aras ◽  
Muhammed Karabulut ◽  
Asgar Kayan

Abstract A Schiff base tin (IV) compound was synthesized by reactions between 2-((E)-(p-tolylimino)methyl)phenol (TIMPH) and butyltin trichloride in 2:1 mole ratio in ethanol at room temperature. [SnBuCl3(TIMPH)2] was characterized by FT-IR, 1H-NMR, 13C-NMR spectroscopy, elemental analysis, and mass spectrometry. Optimization of Murexide dye from aqueous solution was performed by examining; effect of contact time, initial pH, adsorbent amount, initial dye concentration and temperature on the tin adsorbent. The highest adsorption recovery value of was 98.00% and the adsorption capacity was 248.8 mg/g at the end of 20 minutes at 100 mg/L dye concentration while the temperature was 25°C and the pH was 3. Langmuir, Freundlich, and Temkin adsorption isotherms were calculated at 25 ºC. The highest R2 value was found 0.099 for the Langmuir isotherm model. The adsorption characteristics of murexide dye showed that adsorption kinetic obeyed the pseudo-second-order kinetics, and the thermodynamic data suggested the spontaneous and exothermic process.


2019 ◽  
Author(s):  
Nancy Watfa ◽  
Weimin Xuan ◽  
Zoe Sinclair ◽  
Robert Pow ◽  
Yousef Abul-Haija ◽  
...  

Investigations of chiral host guest chemistry are important to explore recognition in confined environments. Here, by synthesizing water-soluble chiral porous nanocapsule based on the inorganic metal-oxo Keplerate-type cluster, {Mo<sub>132</sub>} with chiral lactate ligands with the composition [Mo<sub>132</sub>O<sub>372</sub>(H<sub>2</sub>O)<sub>72</sub>(<i>x-</i>Lactate)<sub>30</sub>]<sup>42-</sup> (<i>x</i> = D or L), it was possible to study the interaction with a chiral guest, L/D-carnitine and (<i>R</i>/<i>S</i>)-2-butanol in aqueous solution. The enantioselective recognition was studied by quantitative <sup>1</sup>H NMR and <sup>1</sup>H DOSY NMR which highlighted that the chiral recognition is regulated by two distinct sites. Differences in the association constants (K) of L- and D-carnitine, which, due to their charge, are generally restricted from entering the interior of the host, are observed, indicating that their recognition predominantly occurs at the surface pores of the structure. Conversely, a larger difference in association constants (K<i><sub>S</sub></i>/K<i><sub>R</sub></i> = 3) is observed for recognition within the capsule interior of (<i>R</i>)- and (<i>S</i>)-2-butanol.


Molecules ◽  
2021 ◽  
Vol 26 (7) ◽  
pp. 1897
Author(s):  
Hideyasu China ◽  
Nami Kageyama ◽  
Hotaka Yatabe ◽  
Naoko Takenaga ◽  
Toshifumi Dohi

We report a convenient and practical method for the preparation of nonexplosive cyclic hypervalent iodine(III) oxidants as efficient organocatalysts and reagents for various reactions using Oxone® in aqueous solution under mild conditions at room temperature. The thus obtained 2-iodosobenzoic acids (IBAs) could be used as precursors of other cyclic organoiodine(III) derivatives by the solvolytic derivatization of the hydroxy group under mild conditions of 80 °C or lower temperature. These sequential procedures are highly reliable to selectively afford cyclic hypervalent iodine compounds in excellent yields without contamination by hazardous pentavalent iodine(III) compound.


2021 ◽  
Author(s):  
Ping-Ru Su ◽  
Tao Wang ◽  
Pan-Pan Zhou ◽  
Xiao-Xi Yang ◽  
Xiao-Xia Feng ◽  
...  

Abstract Design and engineering of highly efficient emitting materials with assembly-induced luminescence, such as room temperature phosphorescence (RTP) and aggregation-induced emission (AIE), have stimulated extensive efforts. Here, we propose a new strategy to obtain size-controlled Eu3+-complex nanoparticles (Eu-NPs) with self-assembly induced luminescence (SAIL) characteristics without encapsulation or hybridization. Compared with previous RTP or AIE materials, the SAIL phenomena of increased luminescence intensity and lifetime in aqueous solution for the proposed Eu-NPs are due to the combined effect of self-assembly in confining the molecular motion and shielding the water quenching. As a proof of concept, we also show that this system can be further applied in bioimaging, temperature measurement and HClO sensing. The SAIL activity of the rare-earth (RE) system proposed here offers a further step forward on the roadmap for the development of RE light conversion systems and their integration in bioimaging and therapy applications.


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