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Preparation method of amino aryloxy rare earth metal amide
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The technology of amino aryloxy rare earth and amino aryloxy rare earth is applied in the field of preparation of amino aryloxy rare earth metal amides, can solve the problems of low yield, troublesome product separation and purification, etc., and achieves high yield, separation and purification. The effect of simple purification and simple process
Inactive Publication Date: 2012-07-25
SUZHOU UNIV
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In this application, amino aryloxy rare earth metal amides are combined with Ln[N(SiMe 3 ) 2 ] 3 (μ-Cl)Li(THF) 3 Synthesized by reaction, the yield of this method is low, only about 40%, and the product separation and purification are troublesome
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Embodiment 1
[0032] Embodiment one: preparation [NO] 2 Nd[N(SiMe 3 ) 2 ] Li 2 (THF) 2 , [NO]=p-X-C 6 h 4 NCH 2 (3-R 2 -5-R 3 -C 6 h 2 -2-O), X is methyl, R 2 , R 3 All are tert-butyl.
[0033] (1) 1.61 g of [NO]H 2 (4.95 mmol) dissolved in tetrahydrofuran, adding n BuLi (4.95 mmol) in hexane, stirred at -10°C for one hour, then added Nd[N(SiMe 3 ) 2 ] 3 (μ-Cl)Li(THF) 3 (2.48 mmol) in tetrahydrofuran solution, the system is blue, stirred and reacted overnight at 50°C;
[0034] (2) Remove the solvent, add 30 milliliters of toluene to heat and extract, centrifuge, transfer the supernatant, add 4.00 milliliters of hexane, concentrate the solution to 12 milliliters, room temperature overnight, separate out 2.48 grams of blue crystals (2.24 mmol), productive rate 90 %.
Embodiment 2
[0035] Embodiment two: preparation [NO] 2 Yb[N(SiMe 3 ) 2 ] Li 2 (THF) 2 , [NO]=p-X-C 6 h 4 NCH 2 (3-R2 -5-R 3 -C 6 h 2 -2-O), X is methyl, R 2 , R 3 All are tert-butyl.
[0036] (1) 0.72 g of [NO]H 2 (2.21 mmol) dissolved in tetrahydrofuran solution, adding n BuLi (2.21 mmol) in hexane, stirred at -10°C for one hour, then added Yb[N(SiMe 3 ) 2 ] 3 (μ-Cl)Li(THF) 3 (1.10 mmol) in tetrahydrofuran solution, the system is yellow, stirred and reacted overnight at 50°C;
[0037] (2) Remove the solvent, add 20 milliliters of toluene to heat and extract, centrifuge, transfer the supernatant, add 3.00 milliliters of hexane, concentrate the solution to 13 milliliters, overnight at room temperature, separate out 1.07 grams (0.94 mmol) of bright yellow crystals, and the yield is 85%.
Embodiment 3
[0038] Embodiment three, preparation [NO] 2 Sm[N(SiMe 3 ) 2 ] Li 2 (THF) 2 , [NO]=p-X-C 6 h 4 NCH 2 (3-R 2 -5-R 3 -C 6 h 2 -2-O), X is fluorine, R 2 , R 3 All are tert-butyl.
[0039] (1) 1.66 g of [NO]H 2 (5.04 mmol) dissolved in tetrahydrofuran solution, adding n BuLi (5.04 mmol) in hexane solution was stirred at -10°C for one hour, and then 2.52 mmol of Sm[N(SiMe 3 ) 2 ] 3 (μ-Cl)Li(THF) 3 tetrahydrofuran solution, the system is yellow, stirred and reacted overnight at 50°C;
[0040] (2) Remove the solvent, add 40 milliliters of toluene to heat and extract, centrifuge, transfer the clear liquid, add 5.00 milliliters of hexane, concentrate the solution to 20 milliliters, and precipitate a large amount of yellow crystals 1.88 grams (2.17 mmoles) at room temperature, the yield is 86 %.
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Abstract
The invention relates to a rare earthmetal compound containing N,O double anion ligands, in particular to a preparation method of an amino aryloxy rare earthmetalamide, which comprises the steps of: 1, reacting an aminophenol ligand with butyl lithium under the condition without oxygen and water in an inertatmosphere; 2, reacting the product obtained in the step 1 with Ln[N(SiMe3)2]3(mu-Cl)Li(THF)3 in a mixed solution of tetrahydrofuran and hexane with a proportion of 10:1-15:1 to prepare [NO]2Ln[N(SiMe3)2] Li(THF)2, wherein Ln is rare earthmetal and is selected from praseodymium, neodymium, samarium, ytterbium and yttrium; [NO] stands for an amino aryloxy ligand and is p-X-C6H4NCH2(3-R2-5-R3-C6H2-2-O), and X is selected from one of hydrogen, C1-C4 saturated alkyl or halogen; and R2 and R3 are respectively selected from one of methyl or tertiary butyl. The method for synthesizing the amino aryloxy rare earth metal amide is suitable for various aminophenol ligands under the mild condition, and has higher yield and simpler separation and purification compared with the method in the Chinese patent application with an application number of 200910181279.
Description
technical field [0001] The invention relates to a rare earth metal complex containing N, O double negativeion ligands, in particular to a preparation method of an amino aryloxy rare earth metal amide. Background technique [0002] Amino aryloxy rare earth metal amides and their catalytic applications are disclosed in the Chinese Invention Patent Application Publication No. 200910181279.7. The general formula of the amino aryloxy rare earth metal amides is [NO] 2 LnN(SiMe 3 ) 2 Li 2 (THF) 2 , where Ln is a rare earth metal, [NO]=p-R 1 -C 6 h 4 NCH 2 (3-R 2 -5-R 3 -C 6 h 2 -2-O), R 1 Selected from: one of hydrogen or C1-C4 saturated alkyl, R 2 and R 3 They are respectively selected from one of methyl group and tert-butyl group; and the application of the compound as a single-component catalyst to catalyze the ring-opening polymerization of L-lactide is disclosed. In this application, amino aryloxy rare earth metal amides are combined with Ln[N(SiMe 3 ) 2 ] 3...
Claims
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