エステル分溜法によるイソニコチン酸-ニコチン酸の分離

概要

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Accurate vapour pressure-temperature curve in the region of pressure of 5〜30 mmHg was prepared for methyl and ethyl esters of nicotinic and isonicotinic acid respectively. From the curve it was calculated that the methyl ester mixture of both acids had a relative volatility of 1.26〜1.24 while the ethyl ester mixture that of 1.15〜1.19. Therefore fractional distillation with an efficient column was supposed to be effective to separate the mixture of these acids. This was realized by the fractional distillation of a synthetic mixture of these acid esters, followed by adsorption analysis in ultraviolet region of each fraction. This method of fractional distillation was also applied with success to mixtures of unknown composition of the esters which were obtained from H_2SO_4-SeO_2 oxidation products of some crude coal tar base fraction. The following results were obtained. (i) The ester mixture obtained from 2,4-lutidine fraction of commercial grade was shown to be consisted of 2 parts of the ester of isonicotinic acid and 1 part of that of nicotinic acid. (ii) That from a commercial quinoline fraction proved to be chiefly composed of the ester of nicotinic acid and only slightly of that of the isonicotinic acid.
宇宙航空研究開発機構の論文
1957-03-15