Analysis of the products from oxidative ammonolysis of 2-methyl-5-ethylpyridine by the gas-liquid chromatography method

Abstract

In the p r e p a r a t i o n of nicotinic acid (I) by the oxidative ammono lys i s of 2 -me thy l -5 -e thy lpyr id ine (II), with subsequent hydro lys i s of the cyanopyr id ines fo rmed [1-3], the v a p o r p h a s e mix ture leaving the oxidative a m monolys i s r e a c t o r may contain, in addition to (II), a l so pyr idine (III), n icot inoni t r i le (IV), 2 c y a n o 5 e t h y l p y r i dine iV), 2 ,5-d icyanopyr id ine (VI), and carbon monoxide and dioxide. In individual c a se s , sl ight amounts of I and of n icot inamide (VII) may be p re sen t . The quanti tat ive analys is of the components of this mix tu re is p e r f o rmed at p r e sen t by the use of g a s l i q u i d ch roma tog raphy (gic) in con]unction with polarography [4, 5]. For ana lys i s , the liquid and solid r eac t ion products a r e t rapped in wate r , and a pa r t of the water solution is anal y z e d b y g l c f o r c o n t e n t o f ( I I V ) . Another par t of the aqueous solution is subjected to alkal ine hydro lys i s and then the content of I and of VI in the fo rm of i soc inchomeronic acid (VIII) is de te rmined polarographica l ly by the method of [5]. This method of ana lys i s often leads to dis tor t ion of the r e su l t s of the polarographic de te r minat ion of content of I and VIII because of the nonspecif ic i ty of the polarographic reduct ion of the pyr id ineca rboxyl ic ac ids [6] and because of par t ia l over lap of the po la rographic waves for reduct ion of I and VIII under the conditions of p e r f o r m i n g the ana lys i s at definite concent ra t ions of components in the mix ture [2].

DOI: 10.1007/BF00757860

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Cite this paper

@article{German2004AnalysisOT, title={Analysis of the products from oxidative ammonolysis of 2-methyl-5-ethylpyridine by the gas-liquid chromatography method}, author={E. N. German and M. Ts. Yanotovskii and L. Ya. Perfil'eva and {\'E}. M. Guseinov}, journal={Pharmaceutical Chemistry Journal}, year={2004}, volume={10}, pages={538-539} }