大位阻富电子金刚烷基有机膦配体的合成  

Synthesis of Bulky Electron-rich Adamantyl Organophosphine Ligands

作　　者：白东亚 贾历力 张垚 石韬 陈辉[1] 刘婷婷 朱向珺[1] BAI Dong-ya;JIA Li-li;ZHANG Yao;SHI Tao;CHEN Hui;LIU Ting-ting;ZHU Xiang-jun(Institute of Chemistry Henan Academy of Sciences,Zhengzhou 450002,Henan,China)

机构地区：[1]河南省科学院化学研究所有限公司,河南郑州450002

出　　处：《合成材料老化与应用》2023年第1期16-19,共4页Synthetic Materials Aging and Application

基　　金：国家自然科学基金(22001060);河南省青年托举人才项目(2021HYTP005);河南省科学院科研开发项目(220603061,221303002,210403023,220603040,200503001)。

摘　　要：以金刚烷为原料,利用傅克酰基化反应得到双(1-金刚烷基)膦酰氯,再用氢化铝锂还原后得到二-1-金刚烷膦,然后与1-碘丁烷成盐得到对空气稳定的正丁基二(1-金刚烷基)膦碘化盐,最后用氢氧化钠释放得到最终产品正丁基二(1-金刚烷基)膦,总收率达72%,产品结构经核磁氢谱、碳谱得以证实,气相色谱检测纯度达98%。Using adamantane as a raw material, the Friedel-Crafts acylation reaction is used to obtain bis(1-adamantyl) phosphonyl chloride, the product was reduced with lithium aluminum hydride to obtain di-1-adamantylphosphine, which was then salted with 1-iodobutane to give an oxidation insensitive of n-butyldi(1-adamantyl) phosphonohydride. Finally, the final product butyldi-1-adamantylphosphine was obtained after the release of sodium hydroxide with a total yield of 72 %. The structure was confi rmed by hydrogen NMR and carbon spectroscopy, and the purity detected by gas chromatography was 98%.

关 键 词：膦配体 二-1-金刚烷基膦氢 正丁基二(1-金刚烷基)膦 合成 

分 类 号：O627.6[理学—有机化学]