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Synthesis, Characterization and Crystal Structure of 2,3,6-Trichloro-5-(trichloromethyl)pyridine
Corresponding Author(s) : Zhao-Sheng Cai
Asian Journal of Chemistry,
Vol. 26 No. 1 (2014): Vol 26 Issue 1
Abstract
2,3,6-Trichloro-5-(trichloromethyl)pyridine (TCTCMP) was synthesized from 2-chloro-5-chloromethyl pyridine (CCMP) through two-steps chloridization using chlorine as chlorizating agent. Initially, 2-chloro-5-chloromethyl pyridine was chloridized for 8 h at reflux conditions in the presence of ultraviolet and transformed into 2-chloro-5-(trichloromethyl)pyridine (CTCMP), then CTCMP was chloridized for 6 h at 175 °C with WCl6 as catalyst. The product was characterized by FT-IR, NMR and elemental analysis. The crystal structure of TCTCMP was investigated using X-ray diffraction and SHELXTL97 software and the result indicated that TCTCMP crystallized in the orthorhombic system, space group Pbcm with a = 8.3100(17), b = 17.018 (3), c = 7.3160(15) Å, V = 1034.6 (4) Å3; Z 4.
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- J.A. Okorley and T.J. Dietsche, US Patent 4723019A (1988).
- S.J. Bis, E.J. Canada, D.H. Cooper, C.S. Galka, N. Kirby, D.G. Ouimette, D.E. Podhorez, M. Pieczko, R. Rezac and B.J. Rieder, WO Patent 9833772,A1 (1998).
- O. Werbitzky and P. Studer, US Patent 6022974 (2000).
- H. Ohi, WO Patent 9526340 A1 (1995).
- K. Shiokawa, S. Tsuboi, S. Kagabu and K. Moriya, EP 0163855 (1985).
- M.J. Marinak and J.L. Simonson, WO Patent 000600 (1985).
- A.P. Fung, J.J. Tai and J.W. Ringer, WO Patent 9850362 A1 (1998).
- C.P. Allphin, M.A. DesJardin and A.D. Harley, EP 544267 A1 (1993).
- P.L. Humphreys and T.J. Dietsche, US Patent 4681945 A (1987).
References
J.A. Okorley and T.J. Dietsche, US Patent 4723019A (1988).
S.J. Bis, E.J. Canada, D.H. Cooper, C.S. Galka, N. Kirby, D.G. Ouimette, D.E. Podhorez, M. Pieczko, R. Rezac and B.J. Rieder, WO Patent 9833772,A1 (1998).
O. Werbitzky and P. Studer, US Patent 6022974 (2000).
H. Ohi, WO Patent 9526340 A1 (1995).
K. Shiokawa, S. Tsuboi, S. Kagabu and K. Moriya, EP 0163855 (1985).
M.J. Marinak and J.L. Simonson, WO Patent 000600 (1985).
A.P. Fung, J.J. Tai and J.W. Ringer, WO Patent 9850362 A1 (1998).
C.P. Allphin, M.A. DesJardin and A.D. Harley, EP 544267 A1 (1993).
P.L. Humphreys and T.J. Dietsche, US Patent 4681945 A (1987).