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为了综合利用氯苯硝化生产硝基氯苯的残液“焦油”,以及提高产品质量和对氯苯硝化机理研究提供依据和线索,我们对该“焦油”的组成进行了研究。前文报道三个副产物2-,3-,及4-氯-2′,4′-二硝基二苯胺的分离。本文报道另外两个新的副产物,氯代三硝基二苯胺(1)和(2)的分离和结构鉴定。1 MS的分子离子峰[M]~+338,高分辨质谱测得分子量338.0040,分子式为C_12H_7N_4O_6Cl。对多硝基反应呈紫红色正反应;对Beilstein试验亦呈正反应。其IR显示1340(苯环硝基)、1445、(苯环)和3295(NH)cm~(-1)。[M]~+与[M十2]~+的丰度比为3∶1,示有一氯。NMR双共振去偶测定,当照
In order to comprehensively utilize “tar”, a residual liquid of nitrochlorobenzene produced by nitration of chlorobenzene, and to provide the basis and clues for improving product quality and nitration mechanism of chlorobenzene, we have studied the composition of “tar”. The foregoing reports on the separation of the three by-products 2-, 3-, and 4-chloro-2 ’, 4’-dinitroaniline. This article reports the isolation and structural characterization of two other new by-products, trichloro-dinitroanilines (1) and (2). 1 MS molecular ion peak [M] ~ +338, high-resolution mass spectrometry measured molecular weight of 338.0040, the molecular formula of C_12H_7N_4O_6Cl. On the reaction of the reaction was purple purple positive reaction; Beilstein test also showed a positive reaction. Its IR shows 1340 (benzene ring nitro), 1445, (benzene ring) and 3295 (NH) cm ~ (-1). The abundance ratio of [M] ~ + to [M + 12] ~ + is 3: 1, showing monochloride. NMR double resonance decoupling determination, when according to