双氟磺草胺的合成新工艺  

Discovery of the Novel Synthetic Process of Florasulam

作　　者：高士光 蔡旭阳 薛欢 陶涛 GAO Shiguang;CAI Xuyang;XUE Huan;TAO Tao(Jiangsu Good Harvest-Weien Agrochemical Co.,Ltd.,Jiangsu Qidong 226200,China)

机构地区：[1]江苏好收成韦恩农化股份有限公司,江苏启东226200

出　　处：《现代农药》2020年第6期22-26,54,共6页MODERN AGROCHEMICALS

摘　　要：以2-甲氧基-5-氟尿嘧啶为起始原料,经氯化反应、肼基化反应、环合反应、转位反应、偶联反应和氯氧化反应获得关键中间体2-氯磺酰基-8-氟-5-甲氧基[1,2,4]三唑[1,5-c]嘧啶,随后该关键中间体与N-氯代丁二酰亚胺(NCS)、甲硫醚、3-甲基吡啶和2,6-二氟苯胺通过磺酰胺缩合反应制备得到双氟磺草胺。结果表明,优化后新工艺以2-甲氧基-5-氟尿嘧啶为起始原料,产品总收率48.8%,含量达98.5%,产品结构经核磁确证。该新工艺路线合理,具备反应条件温和、原料易得、产品质量好、总收率高、成本低廉等特点,适合于工业化生产。Using 2-methoxy-5-fluorouracil as the starting material,the key intermediates(2-chlorosulfonyl-8-fluoro-5-methoxy[1,2,4]triazole[1,5-c]pyrimidine)were obtained through chlorination,hydrazylation,cyclization,transposition,coupling and oxychlorination reactions.Then,it was treated with NCS,Dimethyl sulfide,3-methylpyridine and 2,6-difluoroaniline to obtain florasulam by amidation.The total yield was 48.8%based on 2-methoxy-5-fluorouracil,and the purity was 98.5%.Their structures were confirmed by 1H NMR.The process had advantages of reasonable process,mildreaction conditions,easy availability of materials,high product quality,high yield and low cost,which was suitable for industrialized production.

关 键 词：双氟磺草胺 2-甲氧基-5-氟尿嘧啶 磺酰胺缩合反应 合成 

分 类 号：S482.46[农业科学—农药学]