Font Size: a A A

Synthesis, Structure And Reactivity Of Organolanthanide Bromide Supported By Salicylaldiminato And 2-(1-(2-ethylamino) Pentyl)-phenol Functionalized-NHC Ligand

Posted on:2009-11-01Degree:MasterType:Thesis
Country:ChinaCandidate:J G ZhangFull Text:PDF
GTID:2121360245960247Subject:Organic Chemistry
Abstract/Summary:PDF Full Text Request
We synthesized and characterized neutral lanthanide bromides of L2SmBr (3-1a), L2NdBr (3-1b), L2ErBr (3-1e) and the first cation yttrium bromide [L2Y]+Br- (3-2a) supported by salicylaldiminato functionalized N-heterocyclic carbene according to the protonolysis of Ln-N bonds by imidazolium salt B. We also synthesized the complexes L2NdBr (3-1c) by the metathesis reaction of LLi and the NdCl3. We synthesized the complexes L'2Li2 (3-3a) and [L'2Yb]+Br- (3-3b) via the new trident NHC ligand which synthesized by the addition reaction of n-Buli and imine. The main results as fellows:1. The amide complex of erbium Li(THF)Er(NiPr2)4 (3-1d) was synthesized by the reaction of LiNiPr2 with ErCl3 in the molar ratio of 4:1 and was characterized by X-ray diffraction.2. Reaction of Li(THF)Ln(NiPr2)4 (Ln = Nd, Sm) with imidazolium salt B in the molar ratio of 1:2 at -40°C, gave the complexes L2NdBr (3-1b) and L2SmBr (3-1a). Reaction of imidazolium salt B with n-BuLi in the molar ratio of 1:2, then react with 1/2 equiv NdCl3 at 25°C, also gave the complexes L2NdBr (3-1c). All complexes were characterized by elemental analysis and X-ray diffraction.3. Reaction of Li(THF)Er(NiPr2)4 with imidazolium salt B in the molar ratio of 1:2 at -50°C, gave the corresponding complexes L2ErBr (3-1e) which was the first NHC late lanthanide halide and the first crystal structure of an NHC Er halide.4. Reaction of Li(THF)Y(NiPr2)4 with imidazolium salt B in the molar ratio of 1:2 at -78°C, gave the complexes [L2Y]+Br- (3-2a) which was the first cation NHC yttrium bromide. It was fully characterized by elemental analysis, 1H NMR and 13C NMR, X-ray diffraction. 5. By using the addition reaction of n-Buli and imine in at -78°C, we gave the NHC lithium complex L'2Li2 (3-3a) which was fully characterized by elemental analysis, 1H NMR and 13C NMR, X-ray diffraction.6. Reaction of L'2Li2 (3-3a) with YbCl3 in the molar ratio of 1:1 at room temperature, gave the corresponding cation NHC ytterbium bromide [L'2Yb]+Br- (3-3b). The complexes was characterized by elemental analysis and X-ray diffraction.
Keywords/Search Tags:salicylaldiminato, 2-(1-(2-ethylamino)pentyl)phenol, N-heterocyclic carbene, lanthanide, bromide, synthesis
PDF Full Text Request
Related items