匡婷中期论文(最终定稿)new

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1、学科分类号本科生中期水平实验论文题目（中文）：O-磺酰基肟的制备（英文）：ThepreparationofO-tosyloxime姓名：匡婷学号：2009140221院（系）：化学化工学院专业、年级：化学教育2009级指导教师：邓桂胜副教授二零一二年四月目录中英文摘要·····································································31、前言·······································································

2、···42、实验部分···································································8（1）原料与仪器·····················································8（2）分析测试条件····················································9（3）典型实验分析·······················································93、产品结构分析····

3、·······················································104、实验小结·······························································10参考文献·····································································12O-磺酰基肟的制备姓名：匡婷学号：2009140221指导老师：邓桂胜专业：化学教育专业年级：2009级摘要用呋喃肟与对甲基苯磺酰氯在KI、Ag2O及T

4、HF条件下，避光进行搅拌反应22h后,得到的生成物进行萃取旋蒸得到粗产品，分别用不同比例的石油醚与乙酸乙酯的混合液作为洗脱剂进行硅胶层析柱进行柱层析分离，减压旋蒸得到纯品，并对其进行核磁分析。关键词O-磺酰基肟；呋喃肟；对甲基苯磺酰氯ThepreparationofO-tosyloximeTingKuangGrade:2009Major:chemicalteachingAbstrate:Thereactionofp-methylbenzenesulfonylchloridewithfuraloximeaffordedO-tosyloximeinthep

5、resenceofKI,Ag2OinTHFinblackfor22hours.Themixturewasconcentratedinvacuo.Theresiduewaspurifiedbysilicagelcolumnchromatograph.Concentratingthemixturegaveapureproduct.ThisproductwascharacterizedbyNMR.Keywords:O-tosyloxime;furaloxime;p-methylbenzenesulfonylchlorideO-磺酰基肟的制备1、引言N-磺酰亚

6、胺已被证明是一种很有实用价值的有机合成中间有体，因为它们是少数能够独立稳定的能进行加成反应的缺电子亚胺。为了满足各种不足有机合成反应的需要，人们已经研究发展了多种合成磺酰亚胺的方法。但作为N-磺酰亚胺的类似物，O-磺酰基肟由于其化学不稳定性，很少应用于有机合成中，并且其有效的制备方法也很少见于报道。但是，O-磺酰基肟作为一种亲电试剂，它的制备方法同样值得我们深入研究。已有少量文献报道了O-磺酰基肟在有机合成中的应用。S.ShaukatHusain等人报道了用酮式肟与对甲苯磺酰氯反应生成[1]3H-diazirine的衍生物，取得了较好的结果（见图1-1

7、）[2]MohammadNavidSoltaniRad（见图1-2）和Hossein[3]A.Oskooie（见图1-3）分别用O-磺酰基肟作原料合成了芳基氰，均取得了较好的实验结果。O-磺酰基肟既然能够成功应用于有机合成上，那么就值得我们深入研究它的相关性质。而作为应用的一个重要前提就是简单有效的制备O-磺酰基肟。由此，O-磺酰基肟的制备就成为我们首先要探讨的课题。O-磺酰基肟的合成多见于α-CF3羰基化合物形成的肟与对甲苯[4][5]磺酰氯反应。Chen-YuJiao（见图1-4）和DavidP.Smith（见图1-5）对此类反应进行了研究，但是局

8、限于制备O-磺酰基酮肟OHNCH2OSitButBuCF3iPr2NEt,4-DMAPTsCl