论文部分内容阅读
标题化合物(B2055)是具有较高原卟啉原氧化酶抑制剂除草活性的N-苯基酞酰亚胺类新化合物,合成该化合物的关键步骤是2-[7-氟-4-(丙-2-炔基)-3-氧-3,4-二氢-2H-苯并噁嗪[b][1,4]-6-基]-4,5,6,7-四氢-2H-异吲哚-1,3-二酮(丙炔氟草胺,flumioxazin)的碘化。为寻求更经济和可工业化的合成路线,考察了不同的碘化剂、溶剂、原料配比、反应温度及反应时间对丙炔氟草胺的转化率和产品B2055收率的影响,在以醋酸为溶剂,氯化碘为碘化剂,原料丙炔氟草胺与氯化碘的物质的量比为1∶3,反应温度为20℃,反应时间为60 min的工艺条件下,原料丙炔氟草胺转化率为92.2%,产品B2055收率为90.7%。
The title compound (B2055) is a novel N-phenylphthalimide compound with a higher herbicidal activity of a protoporphyrinogen oxidase inhibitor. The key step in the synthesis of this compound is 2- [7-fluoro-4- 2-ynyl) -3-oxo-3,4-dihydro-2H- benzoxazine [b] [1,4] -6-yl] -4,5,6,7-tetrahydro-2H- Iodination of isoindole-1, 3-dione (flumioxazin). In order to seek a more economical and industrially feasible synthesis route, the effects of different iodination agents, solvents, raw material ratio, reaction temperature and reaction time on the conversion of propy fluroamide and the yield of product B2055 were investigated. As solvent, iodine iodide as iodinating agent, raw material propyne and iodine chloride material ratio of 1: 3, the reaction temperature is 20 ℃, the reaction time is 60 min process conditions, the raw material propyne The conversion of flurotripht was 92.2% and the yield of product B2055 was 90.7%.