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1,3-二叔丁基-5,5-二硝基嘧啶烷(3)是混合炸药含能增塑剂1,3,5,5-四硝基-1,3-二氮杂环环己烷的关键硝化前体.通过研究3的合成反应机理,目的是为制备1,3,5,5-四硝基-1,3-二氮杂环环己烷的工艺优化提供理论依据.以2,2-二硝基-1,3-丙二醇(1)、甲醛和叔丁胺为原料,通过Mannich缩合反应得到1,3-二叔丁基-5,5-二硝基嘧啶烷.采用同位素示踪技术以及分离关键中间体对反应机理进行推测.以氘代甲醛、1和叔丁胺缩合得到氘标记的3,1HNMR和MS分析结果表明:在反应过程中1首先解离生成偕二硝基甲烷和甲醛,小分子碎片随机组合生成了3.分离出了关键中间体1-叔丁氨基-2,2-二硝基乙烷.根据所获得的证据,推断了3的合成反应机理.
1,3-Di-tert-butyl-5,5-dinitropyrimidine (3) is a mixed explosive energy-containing plasticizer 1,3,5,5-tetranitro-1,3-diazacyclic ring Hexane key nitration precursor.Through the study of the synthesis reaction mechanism of 3, the purpose is to provide a theoretical basis for the preparation of 1,3,5,5-tetranitro-1,3-diazacyclohexane process optimization. The 1,3-di-tert-butyl-5,5-dinitropyrimidine was obtained by the Mannich condensation reaction using 2,2-dinitro-1,3-propanediol (1), formaldehyde and t-butylamine as raw materials. Tracer technology and separation of key intermediates to predict the reaction mechanism.Deuterial formaldehyde, 1 and tert-butylamine condensation of deuterium labeled 3,1HNMR and MS analysis results show that: in the reaction process first dissociation to generate gem dinitromethane And formaldehyde, small molecular fragments randomly generated 3. Isolated the key intermediate 1-tert-butylamino-2,2-dinitroethane.According to the evidence obtained, infer the synthesis mechanism of 3.