新烟碱类农药中间体乙酰基恶二嗪的合成

Synthesis of 3-Acetyl-4-nitroimino-perhydro-1,3,5-oxadiazine as an Intermediate for New Nicotinyl Pesticides

对农药重要中间体乙酰基-4-硝基亚氨基-1,3,5-恶二嗪的合成进行了研究,探讨了溶剂、时间、温度、物料配比等因素对反应收率的影响。最佳反应条件为1mol4-硝基亚氨基-1,3,5-恶二嗪与1.2mol乙酰氯以DMF为溶剂、在5℃￣10℃下反应10h,收率80%。并得到了与文献报道理化性质完全不同的产物,结构经IR、1HNMR和元素分析确证。

Research was conducted on the synthesis of an important pesticide intermediate, 3-acetyl-4-nitroimino- perhydro-1,3,5-oxadiazine. The influence of several factors on reaction efficiency were determined, including solvent, time, temperature, and component ratios. Optimum reaction conditions were obtained by combining 1 mole of 4- nitroimino-perhydro-1,3,5-oxadiazine with 1.2 mole of acetyl chloride, using DMF as solvent. At 5 to10℃ and a 10- h reaction time, recovery was 80%. The product had chemical and physical properties completely different from analogous compounds previously reported. Chemical structure was confirmed by H NMR, IR, and elemental analysis. 1