新型杀菌剂唑菌酯吡唑环^(14)C标记合成和鉴定  

Synthesis and Identification of ^(14)C Labelled Pyraoxystrobin

作　　者：刘训悦[1] 阚登蕾[1] 丁兴成[1] 

机构地区：[1]浙江大学原子核农业科学研究所,杭州310029

出　　处：《化学学报》2011年第12期1445-1449,共5页Acta Chimica Sinica

基　　金：国家自然科学基金(No.J20080934);教育部博士点基金(No.J20081244);中央高校基本科研业务费专项资金(No.3A6000-172210206);公益性行业(农业)科研专项经费(No.201103007)资助项目

摘　　要：为研究新型杀菌剂唑菌酯在土壤中的代谢途径、作用机理及环境行为,以14C-对氯苯甲酸为原料,通过取代、环化、缩合三步反应合成吡唑环14C标记的唑菌酯.采用高效液相色谱-质谱联用仪(电喷雾离子源)[HPLC-MS(ESI)],质谱法(电子轰击离子源)[MS(EI)],核磁共振氢谱法(1H NMR)验证了其结构,通过HPLC外标法确定其质量纯度大于98%;液相色谱-流动液闪联用仪(HPLC-LSC)和薄层色谱-同位素成像分析法(TLC-IIA)两种方法分析表明,其放射化学纯度大于98%,比活度为(5.042±0.076)mCi/mmol.以总反应收率计,合成反应的化学收率和放化收率均为43.93%.In order to study the metabolism,mode of action and other environmental behaviors of novel fungicide pyraoxystrobin,a 14C labelled pyraoxystrobin was synthesized from 4-chlorobenzoic acid as 14C labeled carbon source via substitution,cyclization and condensation.Its chemical structure was identified by HPLC-MS（ESI）,MS（EI） and 1H NMR,its purity was determinated by HPLC with more than 98% in mass ratio.HPLC-LSC and TLC-IIA determination demonstrated that its radiochemical purity was more than 98% with specific activity of（5.042±0.076） mCi/mmol.According to the total synthetic yield,the total chemical yield and radiochemical yield were both 43.93%.

关 键 词：唑菌酯 14C标记合成 鉴定 杀菌剂 

分 类 号：TQ450.1[化学工程—农药化工]