双吡啶酮缩氨基硒脲的合成工艺改进

目的：改进双（2-吡啶）酮缩-4-烯丙基-3-氨基硒脲（4）和双（2-吡啶）酮缩-4，4-二甲基-3-氨基硒脲（8）的合成工艺。方法以4-烯丙基-3-氨基硫脲为起始原料，经碘甲烷甲基化，硒氢化钠取代，最后与双（2-吡啶）酮脱水缩合制得终产物4；以4，4-二甲基-3-氨基硫脲为起始原料，与双（2-吡啶）酮脱水缩合，再经碘甲烷甲基化，硒氢化钠取代，最终制得终产物8；并优化各步反应条件。结果按照相应的合成路线有效制备了目标化合物4和8，目标化合物与中间体的结构均经1H NMR、MS谱确认。结论优化后的工艺路线具有成本低、操作简便、适合大量制备等优点。

Improved synthesis of dipyridyl thioselenosemicarbazones

Objective To improve the synthesis process of N-allyl-2-(di(pyridin-2-yl)methylene)hydrazinecarboseleno?amide(4)and 2-(di(pyridin-2-yl)methylene)-N,N-dimethylhydrazinecarboselenoamide(8). Methods 4-allyl-3-thiosemicarbazide (1)was the starting material,which reacted with methyl iodide,sodium hydrogen selenide to obtain intermediate 4-allyl-3-selenosemi?carbazide(3). Compound(3)reacted with di-2-pyridyl ketone to obtain the target compound 4. 4,4-Dimethyl-3-thiosemicarbazide was the starting materials,which reacted with di-2-pyridyl ketone to obtain intermediate dipyridyl thiosemicarbazone(6). Compound 6 re?acted with methyl iodide,sodium hydrogen selenide to obtain the target compound 8. We optimized the reaction conditions of each step. Results We synthesized the target compound 4 and 8 according to the respective synthetic route,the structure of the target com?pounds and the intermediates were confirmed by 1H NMR and MS. Conclusion The improved processes are easy to operate,cost-saving and suitable for large scale preparation.