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Title: Synthesis, characterization and thermal decomposition of di-(2,4,6-trimethylanilinium) sulphate
Authors: Kapoor, Inder Pal Singh
Kapoor, Manisha
Singh, Gurdip
Fröhlich, Roland
Keywords: 2,4,6-trimethylaniline
X-ray diffraction
3-Amino-2,4,6-trimethylbenzenesulphonic acid
Issue Date: Aug-2010
Publisher: CSIR
Abstract: Di-(2,4,6-trimethylanilinium) sulphate [2,4,6-TMAS] was synthesized by reaction of 2,4,6-trimethylaniline with concentrated sulphuric acid at room temperature. The crystal structure of this salt was determined using single crystal X-ray diffraction. It crystallizes in orthorhombic space group Pna21, a= 7.7115(1) Å, b= 30.3746 (6) Å, c=16.9251 (3)Å , ==[°]=90°, V=3964.43 (12)A and Z=8. The structure contains 2,4,6-trimethylanilinium ions that share vertices through intermolecular H- bonds with sulphate ions and a water molecule. Notably thermal and microwave heatings of di-(2,4,6-TMA)S have afforded 3-amino-2,4,6-trimethylbenzenesulphonic acid (3-A-2,4,6-TMBSA) with release of a molecule of amine and water. It has been suggested that the proton transfer from anilinium to SO42- ion is a primary and rate controlling step. Further di-(2,4,6-TMA)S and 3-A-2,4,6-TMBSA were characterized by infrared, mass spectrometry, elemental and thermogravimetric- differential scanning calorimetric (TG-DSC) analyses. The mean value for the energy of activation (83.0 kJ mol-1) for the conversion of di-(2,4,6-TMA)S to 3-A-2,4,6-TMBSA has been determined from isothermal thermogravimetry data.
Page(s): 305-310
ISSN: 0975-1017 (Online); 0971-4588 (Print)
Source:IJEMS Vol.17(4) [August 2010]

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