新型除草剂丙酯草醚A环^(14)C均标记合成和鉴定

Radiolabeled Synthesis and Identification of a Novel Herbicide, Pro-pyl4-[2-(4,6-Dimethoxy-2-pyrimidinyloxy)benzylamino]benzoate with All Six Benzoic Ring Carbons Labeled by ^(14)C

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1HNMR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±0.011mCi/mmol.合成的化学收率和放化收率均为53%.

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 spe- cific activity was 1.089±0.011 mCi/mmol. The total chemical yield and radiochemical yield were all 53%.