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化学学报
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化学学报 ›› 2005, Vol. 63 ›› Issue (21): 1999-2003. 上一篇    下一篇

研究论文

新型除草剂丙酯草醚A环14C均标记合成和鉴定

杨征敏1,3，叶庆富2，唐庆红3，吕龙*,3，陈子元2   

  1. (1西北农林科技大学生命科学学院 咸阳 712100)
    (2浙江大学原子核农业科学研究所 杭州 310029)
    (3中国科学院上海有机化学研究所 上海 200032)
  • 投稿日期:2005-05-20 修回日期:2005-07-18 发布日期:2010-12-10
  • 通讯作者: 吕龙

Radiolabeled Synthesis and Identification of a Novel Herbicide, Propyl 4-[2-(4,6-Dimethoxy-2-pyrimidinyloxy)benzylamino]benzoate with All Six Benzoic Ring Carbons Labeled by 14C

YANG Zheng-Min1, 3, YE Qing-Fu2, TANG Qing-Hong3, LU Long*, 3, CHEN Zi-Yuan2   

  1. (1 College of Life Science, Northwest Science and Technology University of Agriculture and Forestry, Xianyang 712100)
    (2 Institute of Nuclear-Agricultural Science, Zhejiang University, Hangzhou 310029)
    (3 Shanghai Institute of Organic Chemistry, Chinese Academy of Sciences, Shanghai 200032)
  • Received:2005-05-20 Revised:2005-07-18 Published:2010-12-10
  • Contact: LU Long

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以U-14C-对氨基苯甲酸为前体, 通过酯化、缩合、还原和取代四步反应获得了A环14C均标记的丙酯草醚, 用PHPLC对其进行纯化. 采用HPLC-MS(ESI), MS(EI)和1H NMR验证了其结构, 通过HPLC(外标法)确定其化学纯度大于98%; HPLC-LSC和TLC-IIA两种方法分析表明, 其放射化学纯度大于98%, 其比活度为1.089±0.011 mCi/mmol. 合成的化学收率和放化收率均为53%.

关键词: 丙酯草醚(A-环-U-14C), 放射性标记合成, 鉴定, 除草剂

A radiochemical, propyl 4-[2-(4,6-dimethoxy-2-pyrimidinyloxy)benzylamino]benzoate with all six benzoic ring carbons labeled by 14C was made from 4-aminobenzoic acid with all six benzoic ring carbons labeled by 14C through esterification, condensation, reduction and substitution, and purified by preparative HPLC. Its structure was identified by LC-MS and 1H NMR. HPLC test showed its chemical purity exceeded 98%. HPLC-LSC and TLC-IIA demonstrated that its radiochemical purity exceeded 98% and specific activity was 1.089±0.011 mCi/mmol. The total chemical yield and radiochemical yield were all 53%.

Key words: propyl 4-[2-(4,6-dimethoxy-2-pyrimidinyloxy)benzylamino]benzoate with all six benzoic ring carbons l, radiolabelled synthesis, identification, herbicide