五硫化二磷促进醛肟制备伯硫代酰胺的研究  

Synthesis of Primary Thioamides from Aldoximes Mediated by P2S5

作　　者：王耀天 王仪 黄学聪 李江胜 WANG Yao-tian;WANG Yi;HUANG Xue-cong;LI Jiang-sheng(School of Chemistry and Food Engineering,Changsha University of Science&Technology,Changsha 410117,China)

机构地区：[1]长沙理工大学化学与食品工程学院,湖南长沙410117

出　　处：《精细化工中间体》2020年第2期37-40,共4页Fine Chemical Intermediates

基　　金：长沙市科技计划项目(kq1801053);长沙理工大学大学生研究性学习与创新性实验计划项目。

摘　　要：建立了芳香醛肟在五硫化二磷作用下直接转化成伯硫代酰胺的方法,优化工艺条件为:n(肟)∶n(五硫化二磷)=1∶1,反应温度为80℃,干燥苯为溶剂。在此优化条件下,合成了九种伯硫代酰胺,分离收率为74%~90%。研究表明,五硫化二磷在反应中既是脱水剂,亦是硫化试剂;方法操作简单,官能团耐受性好,适合放大生产。A method for the synthesis of primary thioamides from aromatic aldoximes mediated by phosphorous pentasulfide(P2 S5) was established. The optimized reaction conditions were as follows: the molar ratio of oxime to P2S5 of 1∶1;the reaction temperature of 80 ℃;dried benzene as the best solvent. Under the optimal conditions,nine primary thioamides were synthesized in isolated yields of 74%~90%. The results showed that phosphorous pentasulfide served both as a dehydrating reagent and a thionation reagent. In addition, this method has advantages including easy operation, good functional group tolerance, and applicability to large scale production.

关 键 词：硫代酰胺 肟 BECKMANN重排 合成 

分 类 号：O623.626[理学—有机化学]