KI促进乙酰丙酮、CS2与苄氯及其衍生物缩合制备烯酮二硫缩酮类化合物  

KI Promotes Condensation Between Acetylacetone,CS2,Benzyl Chloride and Its Derivatives to Obtain Ketene Dithioacetals

作　　者：李小港 李雪琴 申秀丽[1] 孙岩峰 LI Xiao-gang;LI Xue-qin;SHEN Xiu-li;SUN Yan-feng(College of Chemistry and Bioengineering,Yichun University,Yichun 336000,China;Technology Center,Zhejiang Jihua Group,Hangzhou 311234,China)

机构地区：[1]宜春学院化学与生物工程学院,江西宜春336000 [2]浙江吉华集团股份有限公司技术中心,浙江杭州311234

出　　处：《化学试剂》2020年第11期1377-1380,共4页Chemical Reagents

基　　金：江西省作物生长发育重点实验室开放基金项目(KFJJ201702)。

摘　　要：以廉价的苄氯及其衍生物为原料代替苄溴与乙酰丙酮、CS2缩合,高产率的合成目标化合物。在室温下,以K2CO3为碱,在N,N-二甲基甲酰胺溶剂中,KI能够有效的促进亲核反应进行,从而提高产物的产率。以4-溴苄氯参与的缩合反应为模式反应,考察了KI对反应的促进作用,20 mol%KI存在下反应12 h,即可得到90%的产率,而无KI时产率仅为69%。KI对于其他苄氯参与的反应同样有效,共合成8个化合物,产率68%~95%,目标产物结构通过核磁和元素分析进行了确证。Using cheap benzyl chloride and its derivatives as raw material,the title compounds were obtained via the condensation between acetylacetone,CS2 with high yield.At room temperature,KI promotes the reaction,which used dimethylformamid as solvent and K2CO3 as base.The condensation between acetylacetone,CS2 and 4-bromobenzyl chloride was used as model reaction,and the promotion of KI for the condensation was investigated.In the presence of 20 mol%KI,the yield was 90%.On the contrary,the product was separated with only 69%yield in the absence of KI.The protocol was also efficient for the condensation of the substituted benzyl chloride,through which 8 target compounds were obtained in 68%~95%yield.The structures of the target products were confirmed by NMR and elemental analysis.

关 键 词：苄氯 烯酮二硫缩酮 KI 晶体结构 缩合反应 

分 类 号：O621[理学—有机化学]