摘要
水合肼和乙酸乙酯肼合生成的乙酰肼光化环合生成甲基噁二唑酮经与氯代丙酮取代生成氧代甲基噁二唑丙酮后和水合肼经开扩环、肼酮缩合生成三嗪酰氨后经酸解、中和生成三嗪胺;3-甲基吡啶氨氧化自制合成烟氰,加氢生成烟醛后在酸性条件下与氨基三嗪酮醛酮缩合制得吡蚜酮。500吨/年生产装置工艺稳定运行总收率50.8%,产品纯度≥98%。
Ethyl acetate and hydrazine hydrate prepared acetic acid hydrazine.Then used phosgene/liquid/solid phosgene to synthesis oxadiazole ketone,oxadiazone was substituted by monochloroacetone to acetonyloxadiazole ketone,then ring expansion and condensation and hydrazinolysis reaction to acetaminotriazone,then hydrolysis with acid and neutralize to aminotriazone,then reacted with hydrogenation reaction product of 3-pyridinecarboxaldehyde from self-made 3-cyanopyridine by ammoxidation from 3-methylpyridine to produce pymetrozine.The synthesis of the intermediates was important,and the side reactions could be restrained by controlling the reactions conditions,the yield and purity of 500t/y production plant were improved to 50.8%and 98%more.
关键词
吡蚜酮
吡嗪酮
高效稻飞虱拒食型杀虫剂
工业化
生产工艺
经济效益
Pymetrozine
High eficient antifeedant insecticide,Triazinone
Industrialization
Productive technology
Economic benefit
