摘要
[目的]研究除草剂氟胺磺隆的合成方法。[方法]以邻甲基水杨酸为原料,经甲酯化、加成、Newman-Kwart重排、氯磺化4步反应得到2-氯磺酰基-3-甲基-苯甲酸甲酯,再与2-氨基-4-二甲胺基-6-三氟乙氧基-均三嗪一步缩合反应生成氟胺磺隆。[结果]在优化的条件下,产物纯度高达99%,总收率57.8%(以邻甲基水杨酸计),产物结构经GC-MS、1H NMR确认。[结论]该工艺原料简单易得,成本较低,而且操作简便、收率高,适宜工业化生产。
[Aims] The objective is to study the synthetic method of triflusulfuron-methyl. [Methods] Triflusulfuronmethyl can be obtained through a condensation reaction of 2-amino-4-dimethylamino-6-trifluoroethoxy sym-triazine and 2-chlorosulfonyl-3-methyl-benzoate, which was synthesized from 3-methylsalicylic acid via methyl, addition, Newman- Kwart rearrangement and chlorosulfonation. [Results] The total yield was 57.8% on 3-methylsalicylic acid under the optimized reaction conditions and purity was as high as 99%. The structure of the end product was confirmed by GC- MS and H NMR. [Conclusions] The method has some advantages of simple and easily available materials, lower costs, simple procedure, and high yield, which is suitable for industrial production.
出处
《农药》
CAS
CSCD
北大核心
2013年第10期723-725,共3页
Agrochemicals
关键词
氟胺磺隆
合成
邻甲基水杨酸
triflusulfuron-methyl
synthesis
3-methylsalicylic acid