水稻田除草剂三唑酰草胺的合成

目的]改进合成工艺,提高总收率。方法]以2,4-二氟苯胺为原料,与溴丙烷发生N上的烷基化反应制得N-异丙基-N-2,4-二氟苯胺,再与固体光气发生酰化反应得到中间体N-异丙基-N-2,4-二氟苯基氨基甲酰氯;以2,4-二氯苯胺为原料,经重氮化,还原反应,得到2,4-二氯苯肼盐酸盐,然后分别与甲醛、氰酸钠和次氯酸反应得到1-(2,4-二氯苯基)1,2,4-三唑-5-酮。最后,N-异丙基-N-2,4-二氟苯基氨基甲酰氯和1-(2,4-二氯苯基)-1,2,4-三唑-5-酮反应得到目标产物三唑酰草胺。结果]经1H NMR光谱鉴定,产品结构与三唑酰草胺结构一致。结论]该工艺简单经济,条件温和,适合工业化生产。

Synthesis of Herbicides Ipfencarbazone

Aims] For improving synthetic process and raising yield. Methods] N-Isopropyl-2,4-difluoroaniline which was prepared by alkylation of 2,4-difluoroaniline with 2-bromopropane on N atom, reacted with solid phosgene to obtain the intermediate of N-isopropyl-N-2,4-difluoro phenylcarbamoyl chloride. The 2,4-dichlorophenylhydrazine hydrochloride was synthesized through diazotization with sodium nitrite, followed by reduction with sodium sulfite using2,4-dichloroaniline as raw material, then it reacted respectively with formaldehyde, sodium cyanate and hypochlorous acid to obtain the 1-(2,4-dichlorophenyl)-1,2,4-triazole-5-one, finally, N-isopropyl-N-2,4-difluorophenylcarbamoyl chloride reacted with 1-(2,4-dichlorophenyl)-1,2,4-triazole-5-one to obtain the target product ipfencarbazon. Results] The product obtained was identified by1 H NMR, and the structure was consistent with that of triazolamide. Conclusions] This process is simple, warm and economical, which is suitable for industrial scale manufacture.