SYNTHESIS, POTENTIOMETRIC TITRATIONS, AND SPECTRA OF PYRAZOLONES

1953 ◽  
Vol 31 (11) ◽  
pp. 1025-1039 ◽  
Author(s):  
Paul E. Gagnon ◽  
Jean L. Boivin ◽  
René J. Paquin

Monosubstituted benzoylacetic esters, obtained by condensation of n-alkyl halides with ethyl benzoylacetate, were reacted with hydrazine and phenylhydrazine to give 3-phenyl and 1,3-diphenyl 5-pyrazolones monosubstituted in position 4 by alkyl radicals R (R = H, CnH2n+1(n-1 to 10), and C6H5CH2.). The dissociation constants of the pyrazolones were determined by potentiometric titrations. A study was made of the ultraviolet absorption spectra in both neutral and acid medium and of the infrared absorption spectra. X-ray powder diffraction patterns and data of the pyrazolones were obtained.

1956 ◽  
Vol 34 (4) ◽  
pp. 530-540 ◽  
Author(s):  
Paul E. Gagnon ◽  
Jean L. Boivin ◽  
Yvon Laflamme

Monosubstituted benzoylacetic esters C6H5COCH(R)CO2C2H5 (R = H, CnH2n+1 (n = 1 to 9), and C6H5CH2) obtained by the condensation of n-alkyl halides with ethyl benzoylacetate were reacted with o-, m-, and p-chlorophenyl hydrazines to give 1-chlorophenyl-3-phenyl-4-alkyl-5-pyrazolones. Pyrazolones-4-C14 were prepared by the action of the same hydrazines on ethyl benzoylacetate-α-C14 obtained from benzoyl chloride and ethyl malonate-2-C14. Their activities were 801, 894, and 847 c./min. respectively. The ultraviolet and infrared absorption spectra of all the pyrazolones were determined and the most probable structures ascribed to the compounds.


1980 ◽  
Vol 45 (12) ◽  
pp. 3262-3265 ◽  
Author(s):  
Alexander Muck ◽  
Jindřich Čáp ◽  
Bohumil Hájek

The system Ag3PO4-Ag3AsO4 has been studied by X-ray analysis of the powder samples and infrared absorption spectra. Formation of cubic mixed crystals of the substitution type has been found within the whole concentration range. For the tetrahedral anions at the site T(2) lowering of the site-symmetry to the effective site-symmetry C3 has been found on the basis of the site-and factor-group analyses of the space group Td4.


1970 ◽  
Vol 14 ◽  
pp. 57-66 ◽  
Author(s):  
Racquel Z. LeGeros ◽  
John P. LeGeros ◽  
Otto R. Trautz ◽  
W. Paul Shirra

AbstractThe incorporation of carbonate in the apatite causes a decrease in crystallite size as demonstrated in precipitated apatites prepared at 37°C. Carbonate disturbs the crystallization of the growing apatite crystallites to such an extent that materials with more than 15 wt% CO3 gives an ‘amorphous’ x-ray diffraction pattern. The incorporation of carbonate in precipitates prepared at 100°C. causes a shortening of the a-axis and a lengthening of the c-axis which is proportional to the carbonate content, supporting the concept that in these apatites, CO3 substitutes for PO4 (11). X-ray diffraction linebroadening studies of CO3-apatites precipitated at 100°C and electron micrographs show that the size and shape of the crystallites change from long needles to smaller rods to tiny spheroids, depending upon the amount of CO3. Carbonate causes the bonding in the apatite to become weaker and more isotropic, which results in the small spheroidal crystals.This paper reports the effect of carbonate on lattice parameters and morphology of carbonate-apatites which have been prepared by the conversion of rnonetite, CaHPO4 in hot carbonate solutions. The structural effects of CO3 on the apatite is further reflected by the modification of the vibrations of the PO4 groups in the infrared absorption spectra. The morphology of ‘amorphous’ CO3- containing apatitic precipitates and that of CO3∼apatite with high CO3 content (prepared at 100°C) is similar, i.e., spheroidal in shape, but greatly differing in crystallite size.


1960 ◽  
Vol 38 (12) ◽  
pp. 2349-2358 ◽  
Author(s):  
G. D. Thorn

An attempt has been made to answer several apparent objections to the structure ethylene-thiuram monosulphide assigned to the monomeric material of formula C4H6N2S3 obtained by air oxidation of disodium ethylenebisdithiocarbamate. Comparison of the ultraviolet and infrared absorption spectra, potentiometric titrations, and biological assays of the compound and several heterocyclic and other compounds containing the N–C–S grouping has eliminated two possible alternative structures containing thiadiazolidine and dithiazolidine ring systems and has led to the conclusion that the original assignment of structure was correct.


1970 ◽  
Vol 48 (16) ◽  
pp. 2637-2639 ◽  
Author(s):  
L. K. Walford ◽  
Richard J. Blattner ◽  
Stephen Feldman ◽  
R. L. Bain

The crystal structures of (C6H5)4AsBF4, (C6H5)4AsPF6, (C6H5)4AsAsF6, and (C6H5)4AsSbF6 have been studied by X-ray diffraction. The unit cells are all tetragonal. The fluoroborate compound is probably isostructural with (C6H5)4AsFeCl4. The other three compounds are almost isostructural with (C6H5)4AsFeCl4, the only change being the accommodation of the dipyramidal PF6− ion in the space group [Formula: see text] (No. 82). Infrared absorption spectra are in general agreement with previous work on tetraphenylarsonium halides and compounds with hexafluoro Group VA ions. It is concluded that crystal field effects for this series of salts do not markedly affect the vibrational spectra.


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