Amino aryloxy rare earth metal complex, preparation thereof and application thereof
An amino aryloxy rare earth, metal complex technology, applied in organic compounds/hydrides/coordination complex catalysts, compounds containing periodic table Group 3/13 elements, chemical instruments and methods, etc. The problems of synthesis and low catalytic performance of aryloxy rare earth metal complexes can achieve the effect of high yield, convenient method and high activity.
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Embodiment 1
[0034] Example 1: {[NO]LaN(TMS) 2 } 2 (R 1 = R 2 = Bu t )Synthesis
[0035] Ligand [NO]H 2 (0.68 g, 2.00 mmol) of toluene solution was added to La(N(TMS) 2 ] 3 (μ-Cl)Li(THF) 3 In the toluene solution (1.75 g, 2.00 mmol), the colorless clear solution gradually changed to yellow turbid solution, and the solution was stirred at 80°C overnight. Centrifuge while hot, remove the precipitate, transfer the clear solution, and concentrate. After a few days at room temperature, 1.39 grams of colorless crystals are precipitated, and the yield is 95%. {[NO]LaN(TMS) 2 } 2 Infrared spectrum (KBr, cm -1 ): 3635(s), 2945(s), 2336(m), 1604(s), 1535(s), 1458(m), 1358(m), 1290(w), 1200(s), 1150(w ), 1086(s), 1083(m), 860(w), 836(s), 745(s), 553(m). NMR: 1 H NMR (400 MHz, d 8 -THF): 7.05-7.20(m, Ar-CH 3 ); 7.02-7.04(m, 2H, Ar); 6.98-7.02(m, 2H, Ar); 6.66-6.71(m, 4H, Ar); 6.42-6.45(m, 2H, Ar); 6.01-6.06( m, 2H, Ar); 4.18(s, 4H, CH2); 4.10(s, 6H, OCH3); 2.30(s, Ar-CH3); 1.44(s, 18H, tBu-Ar); 1....
Embodiment 2
[0036] Embodiment 2: {[NO]NdN(TMS) 2 } 2 (R 1 = R 2 = Bu t )Synthesis
[0037] Ligand [NO]H 2 (0.68 g, 2.00 mmol) of toluene solution was added to Nd(N(SiMe 3 ) 2 ] 3 (μ-Cl)Li(THF) 3 In the toluene solution (1.76 g, 2.00 mmol), the clear blue-purple solution gradually turned into a blue-green turbid solution, and the solution was stirred at 80°C overnight. Centrifuge while hot, remove the precipitate, transfer the clear solution, and concentrate. After a few days at room temperature, 1.37 g of blue crystals are precipitated, and the yield is 93%. {[NO]NdN(TMS) 2 } 2 Infrared spectrum (KBr, cm -1 ): 3650(s), 2958(s), 2466(s), 1640(s), 1508(s), 1458(s), 1419(m), 1358(m), 1300(w), 1245(s) ), 1172(w), 1122(s), 1022(m), 883(w), 836(s), 748(s), 532(m). Elemental analysis: C, 57.21%; H, 7.69%; Nd, 19.45%; N, 3.76%. The above data proves that the target compound was successfully prepared.
Embodiment 3
[0038] Example 3: {[NO]SmN(TMS) 2 } 2 (R 1 = Bu t , R 2 = Me) synthesis
[0039] Ligand [NO]H 2 (0.65 g, 2.00 mmol) of toluene solution was added to Sm(N(SiMe 3 ) 2 ] 3 (μ-Cl)Li(THF) 3 In the toluene solution (1.77 g, 2.00 mmol), the color of the solution gradually changed from yellow to red turbid solution, stirred at 70°C overnight. Centrifuge while hot, remove the precipitate, transfer the clear liquid, and concentrate. After a few days at room temperature, 1.34 g of red crystals are precipitated, and the yield is 90%. {[NO]SmN(TMS) 2 } 2 Infrared spectrum (KBr, cm -1 ): 3700(s), 2954(s), 2450(s), 1600(s), 1477(s), 1358(m), 1230(m), 1246(s), 1169(w), 1122(s) ), 984(m), 933(s), 836(s), 744(s), 602(s), 521(m). Elemental analysis: C, 56.66%; H, 7.54%; Sm, 20.21%; N, 3.69%. The above data proves that the target compound was successfully prepared.
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