Study of the alkaline hydrolysis of ethyl 2-(1,2-benzisothiazolin-3-ylidene)cyanoacetate: spectroscopic properties, and X-ray crystal analysis of 2,4-bis-(1,2-benzisothiazol-3-yl)3-aminocrotononitrile–dimethylformamide

Author(s):  
E. Gaetani ◽  
T. Vitali ◽  
A. Mangia ◽  
M. Nardelli ◽  
G. Pelizzi
2021 ◽  
Vol 17 ◽  
pp. 983-990
Author(s):  
Ákos Bajtel ◽  
Mounir Raji ◽  
Matti Haukka ◽  
Ferenc Fülöp ◽  
Zsolt Szakonyi

A library of pinane-based 2-amino-1,3-diols was synthesised in a stereoselective manner. Isopinocarveol prepared from (−)-α-pinene was converted into condensed oxazolidin-2-one in two steps by carbamate formation followed by a stereoselective aminohydroxylation process. The relative stereochemistry of the pinane-fused oxazolidin-2-one was determined by 2D NMR and X-ray spectroscopic techniques. The regioisomeric spiro-oxazolidin-2-one was prepared in a similar way starting from the commercially available (1R)-(−)-myrtenol (10). The reduction or alkaline hydrolysis of the oxazolidines, followed by reductive alkylation resulted in primary and secondary 2-amino-1,3-diols, which underwent a regioselective ring closure with formaldehyde or benzaldehyde delivering pinane-condensed oxazolidines. During the preparation of 2-phenyliminooxazolidine, an interesting ring–ring tautomerism was observed in CDCl3.


2021 ◽  
Author(s):  
Ákos Bajtel ◽  
Mounir Raji ◽  
Matti Haukka ◽  
Ferenc Fülöp ◽  
Zsolt Szakonyi

A library of pinane-based 2-amino-1,3-diols, analogues of biologically active sphingosine, was synthesised in a stereoselective manner. Isopinocarveol prepared from (–)-α-pinene was converted to condensed oxazolidin-2-one in two steps by carbamate formation followed by a stereoselective aminohydroxylation process. The relative stereochemistry of the pinane-fused oxazolidin-2-one was determined by 2D NMR and X-ray technics. The regioisomeric spiro-oxazolidin-2-one was prepared in a similar way starting from commercially available (1R)-(–)-myrtenol. Reduction or alkaline hydrolysis of oxazolidines followed by reductive alkylation resulted in primary and secondary 2-amino-1,3-diols, which underwent regioselective ring closure with formaldehyde or benzaldehyde delivering pinane-condensed oxazolidines. During the preparation of 2-phenyliminooxazolidine, an interesting ring–ring tautomerism was observed in CDCl3.


Polymers ◽  
2019 ◽  
Vol 11 (11) ◽  
pp. 1843 ◽  
Author(s):  
Leyre Pérez-Álvarez ◽  
Leire Ruiz-Rubio ◽  
Isabel Moreno ◽  
José Luis Vilas-Vilela

There is currently an increasing interest in the development of polyacrylonitrile (PAN)-based membranes with new and enhanced properties which are of special importance in the processes of pervaporation, purification, and water treatment. Thus, the optimization of the functionalization of PAN membranes and its effect on their morphology, hydrophilicity, and mechanical properties plays an essential role in a wide range of applications. In this paper, the alkaline hydrolysis of asymmetric PAN membranes was investigated in order to get carboxyl-enriched surfaces that are of a great interest for more demanding subsequent modifications. The process was monitored using –C=NH intermediate bonds, which could be observed during the hydrolysis reaction by X-Ray photoelectron spectroscopy (XPS) and Fourier-transform infrared spectroscopy (FTIR) before the formation of carboxyl and amide groups. The amount of introduced carboxylic acid groups could be determined by thermogravimetric analysis (TGA) and by the interaction with toluidine blue O (TBO) dye. Hydrolysis was revealed as a simple way to modulate hydrophilicity (decreasing contact angle from 60 to 0° for reaction times from 0–3 h) and the mechanical properties of PAN membranes.


1996 ◽  
Vol 11 (7) ◽  
pp. 1748-1754 ◽  
Author(s):  
S. Goñi ◽  
C. Andrade ◽  
J. L. Sagrera ◽  
M. S. Hernández ◽  
C. Alonso

In this work a hypothesis to explain the alkaline hydrolysis degradation process of calcium aluminate cement concrete (CACC) is presented. The hypothesis is based on x-ray diffraction (XRD) data of some samples taken from real Spanish CACC structures. The identification from XRD data of a hydrated alkaline aluminate could serve as a guide to differentiate both processes of normal carbonation and alkaline hydrolysis.


TAPPI Journal ◽  
2011 ◽  
Vol 10 (1) ◽  
pp. 17-23
Author(s):  
KEVIN TAYLOR ◽  
RICH ADDERLY ◽  
GAVIN BAXTER

Over time, performance of tubular backpulse pressure filters in kraft mills deteriorates, even with regular acid washing. Unscheduled filter replacement due to filter plugging results in significant costs and may result in mill downtime. We identified acid-insoluble filter-plugging materials by scanning electron microscope/energy-dispersion X-ray spectroscopy (SEM/EDS) and X-ray diffraction (XRD) analysis in both polypropylene and Gore-Tex™ membrane filter socks. The major filter-plugging components were calcium sulfate (gypsum), calcium phosphate (hydroxylapatite), aluminosilicate clays, metal sulfides, and carbon. We carried out detailed sample analysis of both the standard acid-washing procedure and a modified procedure. Filter plugging by gypsum and metal sulfides appeared to occur because of the acid-washing procedure. Gypsum formation on the filter resulted from significant hydrolysis of sulfamic acid solution at temperatures greater than 130°F. Modification of the acid-washing procedure greatly reduced the amount of gypsum and addition of a surfactant to the acid reduced wash time and mobilized some of the carbon from the filter. With surfactant, acid washing was 95% complete after 40 min.


1980 ◽  
Vol 45 (11) ◽  
pp. 2873-2882
Author(s):  
Vladislav Holba ◽  
Ján Benko

The kinetics of alkaline hydrolysis of succinic acid monomethyl and monopropyl esters were studied in mixed aqueous-nonaqueous media at various temperatures and ionic strengths. The results of measurements are discussed in terms of electrostatic and specific interactions between the reactants and other components of the reaction mixture. The kinetic parameters in the media under study are related to the influence of the cosolvent on the solvation sphere of the reactants.


1984 ◽  
Vol 49 (4) ◽  
pp. 936-943 ◽  
Author(s):  
Bohumil Hájek ◽  
Pavel Karen ◽  
Vlastimil Brožek

For the investigation of the products of reaction of yttrium oxide with carbon mixed in various proportions, the chemical and X-ray diffraction methods of analysis were combined with the gas chromatographic analysis of the mixture of hydrocarbons and hydrogen formed on the sample decomposition with water. The carboreduction of Y2O3 was examined at relatively low temperatures, convenient for obtaining the reaction intermediates in higher yields. At 1 600 °C and pressures of 10-3 Pa the reduction of a mixture of Y2O3 with carbon in a stoichiometric ratio of 1 : 7 yields YC2 in equilibrium with 20% of Y2OC phase. At lower carbon contents (down to the Y2O3 : C ratio of 1 : 2) tha fraction of the Y2OC phase increases up to approximately 30%. In addition to Y2O3, the reaction mixture contains also Y2C, Y2OC and a phase giving propyne on hydrolysis. The presence of traces of C3 hydrocarbons and small amounts of methane in the product of hydrolysis of the carbide sample prepared by the carbothermal reduction of the oxide can be explained in terms of the occurrence of the Y15C19 phase, probably substituted in part by oxygen, and of the Y2OC phase. The results are compared with those obtained previously for the Sc2O3 + C system.


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