New approach to the synthesis of substituted 7H‐furo[3,2‐b]pyran‐7‐ones based on 5‐hydroxy‐2‐methyl‐4H‐pyran‐4‐one derivatives

A convenient approach to the synthesis of the previously unknown 7H‐furo[3,2‐b]pyran‐7‐ones based on the intramolecular cyclization of carbonyl derivatives of 5‐hydroxy‐2‐methyl‐4H‐pyran‐4‐one has been elaborated. Key intermediates in the synthesis of the target 7H‐furo[3,2‐b]pyran‐7‐ones are 3‐hydroxy‐6‐methyl‐2‐(2‐oxo‐2‐arylethyl)‐4H‐pyran‐4‐ones. They are formed as a result of multicomponent condensation of 5‐hydroxy‐2‐methyl‐4H‐pyran‐4‐one with arylglyoxals and 4‐methoxyaniline.     

Synthesis of unsymmetrical 2-(2-vinyl-4H-chromen-4-ylidene)malononitrile dyes via Knoevenagel reaction

A series of new chromophores based on 4-(dicyanomethylene)-2-vinyl 4H-chromenes was synthesized and their physical properties (UV–Vis, NMR, mass spectrometry) were studied. The chromophores show moderate or good solubility in organic solvents. Solvatochromism was investigated for compounds in solvents of low (1.4-dioxane, chlorobenzene, methylene chloride) and high polarity (acetone, acetonitrile). The calculations of the first hyperpolarizability (β) was performed using M052X/6-31+G(d) approximation. Chromophore’s molecules are characterized by high calculated values of the first hyperpolarizability (β) that is only 15% lower than that of FTC analogs.     

Application of centrifugation to the large-scale purification of electric arc-produced single-walled carbon nanotubes

We report a further advance in the bulk purification of nitric acid-treated single-walled carbon nanotubes (SWNTs) by use of high-speed centrifugation. We have already shown that low-speed centrifugation is effective in removing amorphous carbon (AC). In these earlier experiments, the AC preferentially suspends in aqueous dispersions on low-speed centrifugation (2000g), leaving the SWNTs in the sediment. In a surprising reversal, we now show that high-speed centrifugation (20000g) of well-dispersed preparations is effective in sedimenting carbon nanoparticles (CNP), while leaving the SWNTs suspended in aqueous media. Taken together, these two techniques allow the bulk scale (10 g) purification of SWNTs by efficiently separating the two main contaminants, in an industrially viable process. We show that the mechanism of these separations is based on the differential charging (zeta-potential) of the AC, CNPs, and SWNTs that comes about during the chemical processing. Due to their more robust structure, nitric acid oxidation leaves the CNPs with a surface charge density lower than that of the SWNTs, and thus the CNPs do not form stable dispersions in aqueous media during high-speed centrifugation. The efficiency of the process was confirmed by the high purification recovery factor (PRF = 90%), which is a measure of the fractional quantity of the product recovered after the purification. We demonstrate that the purity of SWNTs significantly affects their mechanical and electrical properties.     

[1,2,5]Oxadiazolo[3,4-d]pyridazine 1,5,6-trioxides: efficient synthesis via the reaction of 3,4-bis(hydroxyimino)methyl)-1,2,5-oxadiazole 2-oxides with a mixture of concentrated nitric and trifluoroacetic acids and structural characterization

An efficient synthesis of [1,2,5]oxadiazolo[3,4-d]pyridazine 1,5,6-trioxides (1) from 3,4-bis(hydroxyimino)methyl)-1,2,5-oxadiazole 2-oxides using a mixture of concentrated nitric and trifluoroacetic acids has been developed. The scope of the unconventional reaction was established. The 4,7-dinitro[1,2,5]oxadiazolo[3,4-d]pyridazine 1,5,6-trioxide 1f represents a new high energy compound, unfortunately with low thermal stability. The parent [1,2,5]oxadiazolo[3,4-d]pyridazine 1,5,6-trioxide 1c was studied by single-crystal X-ray diffraction analysis which revealed a planar molecule with an unusually long intracyclic NN bond of 1.668(5)?Å and unexpected exo-cyclic bond angles at the nitroxyl nitrogen atoms. In the crystal, the molecules of 1c are bound to each other by strong π-π stacking and CH?O hydrogen bonding interactions into a three-dimensional framework that results in a high crystal density of 1.833?gcm^?3.     

Investigation of furan acetal compounds

New 1,3-dioxanes, which are derivatives of 2-nitro-2-ethylpropane-1,3-diol and aldehydes of the furan series, were synthesized. The nitrodioxanes were reduced by means of sodium amalgam to the corresponding amines. The kinetics of the formation of the nitrodioxanes was studied. The accelerating action of the electron-acceptor diol substituent on the reaction rate was established. The rate constants in the aldehyde series increase on passing from-methylfurfural to-nitrofurfural, and they correlate satisfactorily with Brown's _p ⁺ constants.See [1] for communication IV.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 9, pp. 1159–1162, September, 1972     

Sorbitol-Based Demulsifying Agents and Their Surfactant Properties

Sorbitol-based block copolymers of ethylene and propylene oxides were synthesized and characterized as surfactants and demulsifiers.__________Translated from Zhurnal Prikladnoi Khimii, Vol. 78, No. 6, 2005, pp. 966–971.Original Russian Text Copyright © 2005 by Solodov, Varnavskaya, Khvatova, Fakhrutdinov, Lebedev, Diyarov.     

Electrocatalytic cascade approach to the synthesis of dihydro-2'H,3H-spiro[1-benzofuran-2,5'-pyrimidines]

Chemistry of Heterocyclic Compounds - Electrocatalytic cascade assembly of benzylidenebarbiturates and cyclohexane-1,3-diones in methanol in the presence of sodium bromide as mediator in an...     

Drift Chambers Made of Mylar Tubes with Diameter of 15 mm and Length of up to 2.5 m

The design and the procedures for assembling and testing drift tubes 15 mm in diameter made of 125-µm-thick Mylar film with a double-sided aluminum coating are presented. The technology of assembling three-layer chambers made of such tubes with a length of up to 2.5 m intended for use in experiments at the accelerator facility at the Institute for High Energy Physics of the National Research Center Kurchatov Institute—IHEP is described. Some results obtained during detection of cosmic muon tracks in the chambers are presented.     

Structural transformations and phase transitions in aqueous solutions of gadolinium nitrate in the course of freezing

The microstructure of Gd(NO₃)₃ aqueous solutions in the course of cooling at different rates is investigated using electron paramagnetic resonance. The local concentrations of Gd³⁺ ions in microregions are estimated, the concentration boundary at which the solution is completely vitrified throughout its volume is revealed, and the temperature of vitrification of liquid microregions (eutectic temperature) and the eutectic composition are determined. It is found that the adsorption of Gd³⁺ aqua ions on the capillary surface affects the crystallization of water and the process of concentration of the solute. It is demonstrated that the anomalous experimental dependence δH(C₀), which is observed for vitrified water-glycerol solutions with a uniform distribution of paramagnetic centers over the sample, agrees well with the theoretical curve in the case when allowances are made not only for the dipole-dipole interactions but also for the inhomogeneous broadening of the EPR lines in the spectra with an incompletely resolved fine structure.