Properties of Guanidine rare earth compounds and catalytic
In this paper, single-ion guanidine, guanidine double anion as ligands (L = [iPrNHC (NiPr) (NC6H4p-R)] -, [(NiPr) 2C (NC6H4p-R)] 2 -), synthesis of a series of three guanidine single ion rare earth complexes, three pairs of rare earth ions guanidine / lithium complex. After all these complexes, including X-ray structure analysis, including full characterization. The effects of amines and their guanidine carbodiimide reaction, terminal alkynes and the amidine carbodiimide reaction and the acylation of aldehydes with amines in the catalytic activity, and two single and double anion guanidine guanidine RE / diimine complexes with lithium response. The main results are as follows:
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(1) We use in situ formation of guanidine salt Li [iPrNHC (NiPr) (N (pR) C6H4)] [R =- Cl,-H], Li [CyNHC (NCy) (N (p-Cl) C6H4 )], Na [(iPrN) 2CN (TMS) 2] and Li [(R''N) 2CNR'2] and rare earth chloride exchange reaction occurred three guanidine complexes of rare earth [iPrNHC (NiPr) ( NC6H4p-R)] 3Ln · THF (Ln = La: R =- Cl (3-1),-H (3-2); Ln = Nd: R =- Cl (3-3),-H (3 - 4); Ln = Y, R =- Cl (3-6)), [CyNHC (NCy) (N (p-Cl) C6H4)] 3Nd (3-5), [(iPrN) 2CN (TMS) 2] 3Nd (3-7), [(R''N) 2CNR'2] 3La, R '=- C6H5, R''=- Cy (3-8),-iPr (3-9); R' =- iPr, R''=- Cy (3-10). All of these complexes have been the IR, elemental analysis and other methods of characterization, in which complex 3-1,3-2,3-6,3-8,3-9 and NMR characterization after 3-10, 3 - 1,3-2,3-3,3-4,3-5 and 3-7 after the X-ray single crystal diffraction. 3-1,3-2,3-3,3-4 the molecular structure is similar, is an octahedral cap, which in the past three guanidino lanthanide complexes differ, is the first center rare earth ion complexation with THF three guanidino lanthanide complexes.
(2) We try to use the synthesis of three rare earth complexes guanidine aldehydes catalyzed amidation reaction, the experimental results show that the three guanidino lanthanide complexes under mild conditions in the aldehydes and amines catalyzed amidation reaction, and has a strong substrate flexibility. The results also show the strength and the catalytic activity of the central metal complexes and ligands are relevant for the central metal ion, the activity order: Yb
(3) We try to use the three guanidino lanthanide complexes with terminal alkynes catalyzed carbodiimide reaction of the amidine, guanidine experimental results show that the three complexes can make the reaction conditions more moderate, and high yields are the product. The results also show the strength and the catalytic activity of the central metal complexes and ligands are relevant for the central metal ion, the activity order: Yb
(4) We double-anion guanidine [(NiPr) 2C (N (pR) C6H4)] 2 - [R =- Cl,-H] for the synthesis of the two-anion ligand guanidine RE / lithium complex Ln [( NiPr) 2C (NLi (pR) C6H4)] 3 [R =- Cl, Ln = Nd (4-1), Y (4-2), La (4-3); R = H, Ln = Nd (4 -4)], all of these complexes have been the IR, elemental analysis and single crystal diffraction and other methods of characterization, single crystal diffraction reveals the double-anion of the guanidine Kiki is a μ-η2η1 with rare earth coordination mode, respectively, with lithium bit. After another complex 4-2,4-3 NMR.
(5) We try to double-anion guanidine RE / lithium complex as catalyst the aldehyde and amine amidation reaction, the experimental results show that the double-anion guanidine RE / lithium complexes can make the reaction under mild conditions, and to give products in high yields, and the substrate has a strong adaptability; double anion guanidine RE / lithium complex catalytic activity than the corresponding three-guanidine complexes of rare earth catalytic activity and amino guanidine of lithium or lithium salt catalytic activity and even higher, indicating that the catalyst there is a certain synergy among. The results also show the strength of the catalytic activity of the center of the catalyst metal and ligand are related, for the central metal ion, the activity of the order: Nd> Y, for the ligand, the catalytic activity of the order of [(iPrN) 2C (NC6H4p-Cl)] 2 -> [(iPrN) 2C (NC6H5)] 2 -.
(6) we try to double-anion guanidine RE / lithium complex as catalyst of the amine and two imine forming guanidine reaction, experimental results show that the double-anion guanidine RE / lithium complexes can make the reaction under mild conditions and the product obtained in high yields, and the substrate has a strong adaptability. The results also show the strength and the catalytic activity of the central metal complexes and ligands are relevant for the central metal ion, the activity of the order: La> Nd> Y; for the ligand, the catalytic activity The order is [(iPrN) 2C (NC6H4 p-Cl)] 2 -> [(iPrN) 2C (NC6H5)] 2 -.
(7) we tried to synthesis of two single-ion guanidine [iPrNHC (NiPr) (NC6H4p-Cl)] - guanidine stable rare earth double-anion / lithium complex [iPrNHC (NiPr) (NC6H4p-Cl)] 2Nd [μ-η2η1 (NiPr) 2C (NLi (p-Cl) C6H4)], but not isolated from the product. Our analysis that the activity of target complexes in H (NH) the presence of instability, will be a qualitative solution. Therefore, we tried not to separate the target product, but then add a carbodiimide and its response to the final two single ions isolated by guanidine guanidine odd and even rare-earth ion / Li-diimine complexes and the addition product [RNHCNR (NC6H4p-Cl)] 2Ln [(RN) 2C (NC6H4p-Cl) C (RN) Li] (R = iPr, Ln = Yb (5-1), Sm (5-2), Nd (5 - 3), Y (5-4); R = Cy, Ln = Nd (5-5)). Then we get a new hybrid double-metal complexes as catalyst of the amine and guanidine forming carbodiimide reaction.
