Synthesis of tricyclic 1,4-dihydro-1,4-phosphagermines – trying to establish molecular fencing of reactive centers
作者:Mridhul. R. K. Ramachandran、Surendar Karwasara、Hui Zhu、Gregor Schnakenburg、Rainer Streubel
DOI:10.1039/d4dt00895b
日期:——
Novel 1,4-dihydro-1,4-phosphagermines (A) have been synthesised bearing small N-alkyl substituents, but the N-Mes substituent led finally to a pentacyclic P,Ge-heterocycle (B); the latter was rationalized using DFT theoretical calculations.
The synthesis of tris(pentafluoroethyl)germanium derivatives is described. The reaction of germanium tetrachloride with three equivalents of the pentafluoroethylation reagent LiC2F5 does not lead selectively to the formation of tris(pentafluoroethyl)chlorogermane, (C2F5)3GeCl. Here the introduction of a diethylamino function as a protecting group was beneficial. Thus, treatment of Cl3GeNEt2 with LiC2F5
描述了三(五氟乙基)锗衍生物的合成。四氯化锗与三当量的五氟乙基化试剂LiC 2 F 5的反应不会选择性地导致形成三(五氟乙基)氯锗烷(C 2 F 5)3 GeCl。在此引入二乙氨基官能团作为保护基是有益的。因此,用LiC 2 F 5处理Cl 3 GeNEt 2顺利得到(C 2 F 5)3 GeNEt 2。氨基取代基被卤化物取代是通过与HBr或HCl在数克规模上反应来完成的。(C的组合2 ˚F 5)3 GeCl有Ag 2 CO 3引起了digermoxane的形成[(C 2 ˚F 5)3的Ge] 2 O.一个钝角的Ge-O-Ge中150.2角(1) °是通过X射线衍射确定的。尝试的双氧烷的水解导致前体,(C 2 F 5)3 GeOH和水的平衡混合物。