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JCR 2016
جستجوی مقالات
سه شنبه 29 مهر 1404
Iranian Journal of Chemistry and Chemical Engineering
، جلد ۴۱، شماره ۴، صفحات ۱۲۳۲-۱۲۳۹
عنوان فارسی
چکیده فارسی مقاله
کلیدواژههای فارسی مقاله
عنوان انگلیسی
A Simple Method for the Preparation of 2,4,6-trichloroborazine and Evaluation of 1H-NMR Spectra
چکیده انگلیسی مقاله
The compound 2,3,6-trichloroborazine (TCB) is known as a valuable precursor to prepare boron nitride and various derivatives of borazine. Difficulties in the preparation of TCB via conventional methods on the one hand, and its importance for material science, on the other hand, were our motivations to modify Brown’s method for TCB synthesis. So far, all reports on the synthesis procedure of TCB are based on the use of gaseous BCl
3
with NH
4
Cl powder at 110-130 °C in chlorobenzene requiring complicated low-temperature equipment such as a cold finger condenser, and dry ice-acetone reflux condenser to retain BCl
3
gas in the reaction flask.
According to our study,
using BCl
3
solution in n-hexane was more convenient than using gaseous BCl
3
. The reaction of BCl
3
solution with NH
4
Cl was carried out without loss of BCl
3
. Furthermore, the reduction in the reflux temperature from 130 °C in some previous studies to 86 °C in our study, was a valuable advantage, leading to the release of the coordinated BCl
3
from the adduct complex
[CH
3
CN
·
BCl
3
]
gradually and the prevention of thermal decomposition of TCB, unwanted polymerization reactions and the formation of undesirable products, resulting in the increased reaction yield. TCB was fully characterized by ATR-FTIR,
11
B-,
14
N-, and
1
H-NMR spectroscopic methods.
1
H-NMR spectra of TCB were performed for the first time at various temperatures to elucidate the quadrupole effect of nitrogen, leading to the observation of the proton resonance splitting of the
14
N-H bond by coupling with the
14
N quadrupole nucleus. The broad peak observed at room temperature was clearly split into a triplet at 100 °C due to the long T
qN
and fast molecular motion of TCB molecules. The
14
N-NMR spectrum was also shown for the first time as a broad signal at δ = –271.3 ppm (h
1/2
= 186 Hz).
کلیدواژههای انگلیسی مقاله
Borazine derivatives,Adduct complex,NMR-Spectroscopy,Quadrupole effect,Boron trichloride
نویسندگان مقاله
Aria Norozi |
Chemistry and Chemical Engineering Research Center of Iran, Tehran, I.R. IRAN
Abdul Wahid Mesbah |
Chemistry and Chemical Engineering Research Center of Iran, Tehran, I.R. IRAN
Effat Iravani |
Nuclear Science and Technology Research Institute, Tehran, I.R. IRAN
نشانی اینترنتی
https://ijcce.ac.ir/article_244169_26be573dacf88ef6a424509f4d06da6f.pdf
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