Please use this identifier to cite or link to this item: http://nopr.niscair.res.in/handle/123456789/10073
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
Thermal
Microwave
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 Pna2<sub>1</sub>, <i style="">a</i>= 7.7115(1) Å, <i style="">b</i>= 30.3746 (6) Å, <i style="">c</i>=16.9251 (3)Å , <img src='/image/spc_char/alpha.gif' border=0>=<img src='/image/spc_char/beta.gif' border=0>=<img src='/image/spc_char/gamma.gif' border=0>[°]=90°, <i style="">V</i>=3964.43 (12)A and <i style="">Z</i>=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 SO<sub>4</sub><sup>2- </sup>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<sup>-1</sup>) for the conversion of di-(2,4,6-TMA)S to 3-A-2,4,6-TMBSA has been determined from isothermal thermogravimetry data.
Description: 305-310
URI: http://hdl.handle.net/123456789/10073
ISSN: 0975-1017 (Online); 0971-4588 (Print)
Appears in Collections:IJEMS Vol.17(4) [August 2010]

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