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机构地区:[1]安徽国星生物化学有限公司,安徽杂环化学省级实验室,安徽马鞍山243100
出 处:《广州化工》2016年第20期74-75,126,共3页GuangZhou Chemical Industry
摘 要:采用邻硝基甲苯与N-溴代丁二酰亚胺(简称NBS)为反应原料来合成邻硝基苄溴,系统的考察了原料配比,溶剂种类,反应温度和反应时间对邻硝基溴苄收率和选择性的影响,筛选出合适的反应条件。用IR和1H NMR表征了其结构。结果显示:当以四氯化碳为溶剂,n(邻硝基甲苯)∶n(NBS)=1∶1.03,回流6 h时,邻硝基苄溴的收率为86%,选择性为94.0%。该路线简单经济,条件温和,收率高,适合工业化生产。O-nitrobenzyl bromide could be synthesized by o-nitromethylbenzene and N-bromobutanimide. The process and the influences of factors on the yield and selectivity were studied,the ratio of raw material,solvent,reaction temperature and reaction time and the appropriate reaction conditions were screened out. The structure was confirmed by IR and1 H NMR. The results showed that when n( o-nitromethylbenzene) ∶n( NBS) = 1∶1. 03 and 6 h after refluxing with carbon tetrachloride as solvent,the total yield was 86% and selectivity was 94. 0%. The process exhibited mild reaction conditions and high yield,and was suitable for industrial production.
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