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本文报导了从4-氧-2,2,6,6-四甲基派啶氧化成4-氧-2,2,6,6-四甲基哌啶-1-氧自由基的一个改进方法,它具有收率高、反应时间短的优点。还对4-氧-2,2,6,6-四甲基哌啶-1-氧与羟胺盐酸盐在不同pH条件下的反应进行了研究:在碱性条件(pH 9—11)下得到该自由基的肟,在近中性条件(pH 7—8)下,得到自由基肟的Beckmann重排产物,在酸性条件(pH 2—5)下,得多一非自由基产物的盐酸盐,其分子式为C_9H_(18)N_2O_2·HCl.4-氧-2,2,6,6-四甲基哌啶-1-氧自由基很容易与抗坏血酸反应,被还原为1-羟基-4-氧-2,2,6,6-四甲基哌啶。对几种氮氧自由基在固态的顺磁共振谱及质谱也进行了测定。
This paper reports an improved method for the oxidation of 4-oxo-2,2,6,6-tetramethylpicrine to 4-oxo-2,2,6,6-tetramethylpiperidine-1-oxyl , It has the advantages of high yield, short reaction time. The reaction of 4-oxo-2,2,6,6-tetramethylpiperidine-1-oxide with hydroxylamine hydrochloride at different pH conditions was also studied: under basic conditions (pH 9-11) The free-radical oxime is obtained and Beckmann rearrangement products of the free-form oxime are obtained under near-neutral conditions (pH 7-8), yielding more salt of a non-free-radical product under acidic conditions (pH 2-5) Acid salt, the formula C_9H_ (18) N_2O_2 · HCl 4-oxo-2,2,6,6-tetramethylpiperidine-1-oxyl radical reaction with ascorbic acid easily, is reduced to 1-hydroxy- 4-oxo-2,2,6,6-tetramethylpiperidine. Several kinds of nitrogen and oxygen free radicals in the solid paramagnetic resonance spectroscopy and mass spectrometry were also measured.