Rare-earth metal arylamine group compound as well as preparation method and application thereof
A technology of amino compounds and rare earth metals, applied in the field of rare earth metal aryl amino compounds and their preparation and application, to achieve the effects of convenient product purification, wide applicability, and clear structure
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Embodiment 1
[0041] Embodiment one: preparation (2,6-R 1 2 PhNH) 5 Y Li 2 (THF) 2 (R 1 selected from isopropyl):
[0042] (1) Preparation of 2,6-R 1 2 PhNHLi: adding a tetrahydrofuran solution of n-butyl lithium (14.05 mmol) into a tetrahydrofuran solution of an arylamine compound (14.05 mmol) and reacting for 1 to 3 hours to obtain lithium arylamide.
[0043] (2) 2,6-R 1 2 A THF solution of PhNHLi (14.05 mmol) was added to YCl 3 (0.55g, 2.81mmol) of tetrahydrofuran suspension, stirred at 50°C for about 10 hours, the system turned into a light yellow transparent solution, removed tetrahydrofuran under reduced pressure, added 10mL toluene for extraction twice, centrifuged to remove a little precipitate, and transferred the supernatant , concentrated, and stood at room temperature until colorless crystals precipitated, 2.54 g, yield 80%. Elemental analysis: C, 65.80; H, 8.794; N, 5.772; C68 h 106 Li 2 N 2 o 2 Theoretical value of Y: C, 72.38; H, 9.47; N, 6.21; infrared spectru...
Embodiment 2
[0044] Embodiment two: preparation (2,6-R 1 2 PhNH) 5 SmL 2 (THF) 2 (R 1 selected from isopropyl):
[0045] (1) Preparation of 2,6-R 1 2 PhNHLi: adding a tetrahydrofuran solution of n-butyl lithium (14.05 mmol) into a tetrahydrofuran solution of an arylamine compound (14.05 mmol) and reacting for 1 to 3 hours to obtain lithium arylamide.
[0046] (2) 2,6-R 1 2 A THF solution of PhNHLi (14.61 mmol) was added to SmCl 3 (0.75g, 2.92mmol) in tetrahydrofuran suspension, stirred at 50°C for about 10 hours, the system turned into a light yellow transparent solution, removed THF under reduced pressure, added 10mL toluene for extraction twice, centrifuged to remove a little precipitate, and transferred the supernatant , concentrated, and stood at room temperature until light yellow crystals were precipitated, 2.64 g, yield 76%. Elemental analysis: C, 63.22; H, 8.879; N, 6.141; C 68 h 106 Li 2 N 2 o 2 Sm. Theoretical value: C, 68.64; H, 8.98; N, 5.89; infrared spectrum (...
Embodiment 3
[0047] Embodiment three: preparation (2,6-R 1 2 PhNH) 5 NdL 2 (THF) 2 (R 1 selected from isopropyl):
[0048] (1) Preparation of 2,6-R 1 2 PhNHLi: adding a tetrahydrofuran solution of n-butyl lithium (14.05 mmol) into a tetrahydrofuran solution of an arylamine compound (14.05 mmol) and reacting for 1 to 3 hours to obtain lithium arylamide.
[0049] (2) 2,6-R 1 2 A THF solution of PhNHLi (15.96mmol) was added to NdCl 3 (0.80g, 3.19mmol) of tetrahydrofuran suspension, stirred and reacted at 50°C for about 10 hours, the system became a light yellow transparent solution, removed THF under reduced pressure, added 10mL toluene for extraction twice, centrifuged to remove a little precipitate, and transferred the supernatant , concentrated, and stood at room temperature until a light blue crystal precipitated, 2.83 g, yield 75%. Elemental analysis: C, 66.26; H, 8.787; N, 5.395; C 68 h 106 Li 2 N 2 o 2 Nd. Theoretical value: C, 69.00; H, 9.03; N, 5.92; infrared spectrum...
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