稳定同位素标记3,5-二硝基水杨酰肼-^(15)N_2的合成  

Synthesis of Labeled 3,5-Dinitrosalicyl Hydrazide-^(15)N_2

作　　者：江浙 卢伟京[1,2] 徐仲杰[1,2] 

机构地区：[1]上海化工研究院,上海200622 [2]国家同位素工程技术研究中心-上海分中心,上海200622

出　　处：《精细化工》2014年第6期812-816,共5页Fine Chemicals

摘　　要：提出简便的方法合成3,5-二硝基水杨酰肼-15N2,即以水杨酸为前体,与硝酸钾-15N硝化得到3,5-二硝基水杨酸-15N2,再经过酯化、肼解反应得到目标产物。以消耗K15NO3计算,3,5-二硝基水杨酰肼-15N2的总收率为55.5%。产品结构经质谱和核磁共振波谱等表征确定,15N的同位素丰度为99.2 atom%15N,色谱纯度为97.3%,可作为食品安全领域检测用同位素内标试剂。This article presents an efficient method for the synthesis of 3,5-dinitrosalicyl hydrazide-15 N2 ,with salicylic acid as the common substrate. Nitration of salicylic acid with KNO3-15N provided 3, 5-dinitrosalicylic acid-15N2 and then we got 3,5-dinitrosalicyl hydrazide-15 N2by the esterification and hydrazinolysis reaction. The yield of 3,5-dinitrosalicyl hydrazide-15 N2 was 55.5% based on K15 NO3. The product was confirmed by NMR and LC-MS to be the target compound. Its chemical purity was 97.3% and isotopic enrichment of 15N was 99.2%. It could be used as internal standard in the field of food safety testing.

关 键 词：稳定同位素标记 3 5-二硝基水杨酰肼 兽药残留检测 

分 类 号：TQ455.47[化学工程—农药化工]