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.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2014年第6期812-816,共5页
Fine Chemicals
