Microwave-assisted synthesis and sublimation enthalpies of hemiporphyrazines

2019 ◽  
Vol 23 (03) ◽  
pp. 296-302 ◽  
Author(s):  
Aleksandra S. Kuznetsova ◽  
Nadezhda L. Pechnikova ◽  
Yuriy A. Zhabanov ◽  
Aleksey E. Khochenkov ◽  
Oscar I. Koifman ◽  
...  

It was established that microwave irradiation solvent-free processing of 2,6- diaminopyridine or 1,3-phenylenediamine with phthalonitrile or 4-tert-butylphthalonitrile led to corresponding hemiporphyrazines with sufficiently high yields and a huge reduction in the time required for synthesis, from 8–12 h to 20 min. The data of IR and UV-vis spectroscopies and elemental analysis of the final products were found to be similar to those described in literature. The obtained hemiporphyrazines were characterized by 1H and [Formula: see text]C NMR data. We applied the Knudsen effusion method with mass spectrometric control of vapor composition. The mass spectrometric investigations established that the macrocyclic compounds give a stable stream of particles and their enthalpies of sublimation were estimated by the second law of thermodynamics.

2006 ◽  
Vol 10 (08) ◽  
pp. 1034-1039 ◽  
Author(s):  
Petr Semyannikov ◽  
Tamara Basova ◽  
Sergei Trubin ◽  
Evgeny Kol'tsov ◽  
Igor Igumenov

Mass spectrometric studies of the composition of the gaseous phase for solid compounds of hexadecafluorinated phthalocyanines MPcF 16, M = Cu , Zn , VO and their unsubstituted MPc analogs were performed in a temperature range up to 600°C. It has been shown that phthalocyanines sublime into the form of monomers without thermal decomposition. The vapor pressure of these phthalocyanines was determined as a function of temperature by the Knudsen effusion method, in which the rate of effusion of the equilibrium vapor through a small orifice was measured. The thermodynamic parameters of the sublimation process for phthalocyanines were calculated.


1981 ◽  
Vol 36 (8) ◽  
pp. 913-916 ◽  
Author(s):  
K. F. Zmbov ◽  
A. Neubert ◽  
H. R. Ihle

Abstract The observation of the gaseous BiPb molecule [1,2] suggests the existence of heteronuclear diatomic molecules of lead with the group V-b elements. The present paper reports on the identification of the SbPb(g) molecule and the determination of its dissociation energy by mass spectrometric Knudsen-effusion method.


Author(s):  
P. P. SEMYANNIKOV ◽  
T. V. BASOVA ◽  
V. M. GRANKIN ◽  
I. K. IGUMENOV

Mass spectrometric studies of the composition of the gaseous phase under solid compounds of free phthalocyanine ( H 2 Pc ) and its complexes with aluminium ( AlClPc , AlFPc , ( AlPc )2 O ) and copper ( CuPc ) were performed in the temperature range up to 700 °C. It has been shown that the phthalocyanines sublime in the form of monomers, excluding one aluminium complex. All phthalocyanines under investigation sublime without thermal decomposition until 700 °C. The vapour pressure of these phthalocyanines was determined as a function of temperature by the Knudsen effusion method, in which the rate of effusion of the equilibrium vapour through a small orifice was measured. The thermodynamic parameters of the sublimation process for phthalocyanies were calculated.


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