新型杀菌剂唑菌酯吡唑环14C标记合成和鉴定Synthesisand.PDF

2011 年第69 卷 化 学 学 报 Vol. 69, 2011 第12 期, 1445～1449 ACTA CHIMICA SINICA No. 12, 1445～1449 ·研究论文· 14 新型杀菌剂唑菌酯吡唑环 C 标记合成和鉴定 刘训悦 阚登蕾 丁兴成* (浙江大学原子核农业科学研究所 杭州 310029) 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 1 谱法( 电子轰击离子源)[MS (EI)], 核磁共振氢谱法( H 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%. 关键词 唑菌酯; 14C 标记合成; 鉴定; 杀菌剂 Synthesis and Identification of 14C Labelled Pyraoxystrobin Liu, Xunyue Kan, Denglei Ding, Xingcheng* (Institute of Nuclear-Agricultural Science, Zhejiang University, Hangzhou 310029) Abstract In order to study the metabolism, mode of action and other environmental behaviors of novel 14 14 fungicide pyraoxystrobin, a C labelled pyraoxystrobin was synthesized from 4-chlorobenzoic acid as C labeled carbon source via substitution, cyclization and condensation. Its chemical structure was identified by 1 HPLC-MS (ESI), MS (EI) and H NMR, its purity was determinated by HPLC with more than 98% in mass ratio. HPLC-LSC and TLC-IIA determination demonstrated that its radioche