含不同取代基的钌-锗化合物的合成及表征
Synthesis and Characterization of Ruthenium Germyl Complexes with Various Substituents
田雁 1董睿 1聂鹏 1许波1
作者信息
- 1. 贵州省食品药品检验所 贵阳 550004
- 折叠
摘要
钌-锗化合物(PPh3)(X)RuGeCl2ArTrip(X=H,1;Cl,2;ArTrip=C6H3-2-(η6-Trip)-6-Trip,Trip=2,4,6-iPr3-C6H3)与有机试剂如格氏试剂、LiHBEt3以及萘钠反应实现了锗和钌原子上的取代基团的调控.化合物1与格氏试剂EtMgBr在不同的温度下反应,分别生成(PPh3)HRuGeBr2ArTrip(3)和(PPh3)HRuGeEt2ArTrip(4).化合物1和LiHBEt3反应也生成化合物4,在该反应中LiHBEt3作为乙基转移试剂而不是氢化试剂.此外,化合物1与HBF4反应生成离子型化合物[(PPh3)H2RuGeCl2ArTrip][BF4](5).另外,利用 Na/naphthalene 还原化合物 2 可以得到双羟基化合物(PPh3)HRuGe(OH)2-ArTrip(6),而化合物2与碘单质的反应历经单碘化,形成化合物(PPh3)IRuGeCl2ArTrip(7).所有的化合物都经过详细的核磁谱学和X射线单晶衍射的表征.
Abstract
Reactions of dichlorogermyl ruthenium complexes(PPh3)(X)RuGeCl2ArTrip(X=H,1;Cl,2;ArTrip=C6H3-2-(η6-Trip)-6-Trip,Trip=2,4,6-iPr3-C6H3)with various reagents,including Grignard reagent,LiHBEt3 and Na/naphthalene were investigated,realizing the substituent modulation on Ge and Ru atoms.1 reacted with EtMgBr forming(PPh3)HRu-GeBr2ArTrip(3)and(PPh3)HRuGeEt2ArTrip(4)depending on the reaction temperature.The reaction of 1 with LiHBEt3 also resulted in the formation of 4,where LiHBEt3 acted as ethyl transfer reagent instead of hydrogenation reagent.Additionally,1 reacted with HBF4 afforded ionic product[(PPh3)H2RuGeCl2ArTrip][BF4](5).On the other hand,reduction of 2 with Na/naphthalene produced dihydroxyl complex(PPh3)HRuGe(OH)2ArTrip(6),while the reaction with I2 underwent monoiodination on Ru with the formation of(PPh3)IRuGeCl2ArTrip(7).All compounds were fully characterized by heteronuclear NMR spectroscopy and single-crystal X-ray diffraction.
关键词
钌/锗宾/取代反应/结构Key words
ruthenium/germylene/substitution/structure引用本文复制引用
基金项目
贵州省科技厅项目(黔科合基础-ZK[2021]一般041)
出版年
2024
NETL
NSTL
万方数据