176
L.I. Larina et al. / Journal of Molecular Structure 604 (2002) 165±176
cooled to 08C and the solid formed was ®ltered and
washed on a ®lter with cold acetonitrile. The yield is
3.32 g (90%), it is yellow crystals with melting point
of 188±1908C. IR spectrum (KBr), n, cm21: 3420,
3110, 3000, 1705, 1630, 1505, 1180, 1080, 880.
Found, %: C 50.96; H 6.40; Cl 14.02; N16.08.
C11H16ClN3O2. Calculated, %: C 51.26; H 6.21; Cl
13.78; N16.31.
References
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3.2.9. 1,1-Dimethylhydrazone pyridine-3-aldehyde (9)
It was obtained by the method described in work
[4]. The boiling point is 112±1148C (3 mmHg).
According to the literature [4], the boiling point is
1388C (10 mmHg).
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1570, 1540, 1380, 1060, 670. Found, %: C 37.46; H
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9
37.11; H 4.81; N14.43; I 43.64.
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3.2.11. Pyridinium 1-carboxyethyl-3-(1,1-dimethyl-
hydrazonomethylen) (11)
It was obtained analogously to 9. The yield is 54%.
It is yellow crystals with the melting point of 183±
1858C. IR spectrum (KBr), n, cm21: 3460, 3200,
3060, 1700, 1605, 1550, 1410, 1400, 900, 810, 800,
690. Found, %: C 50.95; H 6.06; Cl 14.11; N15.94.
C11H16ClN3O2. Calculated, %: C 51.26; H 6.21; Cl
13.79; N16.31.
Acknowledgements
The authors are grateful to Dr J.-P. Kintzinger for
fruitful discussions of the present results and his
hospitality in the NMR Laboratory of Condensed
Matter (Universite Louis Pasteur, 4, rue Blaise Pascal,
67000 Strasbourg, France) in the frame of a Post
Doctoral Grant (L.I.L.) from Rhodia. We thank Dr
J.-R. Desmurs (Rhodia Organique, Pharmaceutical
Ingredients, Etoile Part-Dieu, 190, avenue Thiers,
69457 Lyon Cedex 06, France) and Dr G. Dolgushin
(Irkutsk Institute of Chemistry SB RAS, Russia) for
helpful comments.
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