M-methyl pyridine tetrazole copper [I] complex blue-light emitting material and preparation method thereof
A technology of m-picoline tetrazolium copper and picoline tetrazolium copper is applied in the directions of luminescent materials, copper organic compounds, chemical instruments and methods, etc., and can solve problems such as shortage of raw materials, scarcity of content, and difficulty in mining.
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[0031] The present invention provides a kind of preparation method of m-picoline tetrazolium copper [I] complex blue light material (this is the first preparation method), comprising the following steps:
[0032] Step 1: Under an argon atmosphere, [Cu[MeCN] with a molar ratio of 2:2:1 4 ][ClO 4 ], bis[diphenylphosphine]methane, 5-[5-methyl-2-pyridyl]tetrazolium [pytzH for short] in methylene chloride at room temperature and stirred for 2-4 hours to obtain the first reaction mixture .
[0033]Step 2: adding sodium hydroxide in an equimolar amount to the 5-[5-methyl-2-pyridyl]tetrazolium ligand to the first reaction mixture, and continuing to stir and react at room temperature for 1-2 hours to obtain Second reaction mixture.
[0034] Step 3: Evaporate the solvent of the second reaction mixture to dryness, use dichloromethane-n-hexane mixed solvent for recrystallization, filter and recrystallize to obtain a colorless crystalline product, use ether to wash 3-4 times, and obtain...
Embodiment 1
[0045] Under an argon atmosphere, [Cu[MeCN] 4 ][ClO 4 ] (20.9mg, 0.064mmol), bis[diphenylphosphine]methane (24.6mg, 0.064mmol) and 5-[5-methyl-2-pyridyl]tetrazolium (5.2mg, 0.032mmol) in 10mL Stir and react at room temperature in dichloromethane for 3 hours, then add sodium hydroxide (1.28mg, 0.032mmol) to the reaction solution, continue to stir and react at room temperature for 1 hour, then evaporate the solvent to dryness with a rotary evaporator, and dichloromethane (1mL)-n-hexane (10mL) mixed solvent [volume ratio 1:10] for recrystallization. The colorless crystalline product obtained by recrystallization was filtered, washed 3-4 times with 10 mL of ether, and dried in vacuo to obtain a colorless solid product (30.1 mg, 0.013 mmol), with a yield of 81%.
[0046] Elemental analysis calculated value (C 114 h 100 Cl 2 Cu 4 N 10 o 8 P 8 ) as (%): C 59.25, H 4.36, N 6.06; Found: C 59.27, H 4.38, N 6.03.
[0047] X-ray single crystal diffraction: crystal belongs to tri...
Embodiment 2
[0050] Under argon atmosphere, copper perchlorate hexahydrate [Cu[ClO 4 ] 2 ·6H 2 O] (10.4mg, 0.028mmol) and excess copper powder (12.0mg, 0.189mmol) were stirred at room temperature in 5mL acetonitrile for 30 minutes, then added bis[diphenylphosphine]methane (21.5mg, 0.056mmol) in 10mL di Chloromethane solution, continue to stir and react for 1 hour, then add 5-[5-methyl-2-pyridyl]tetrazolium (4.5mg, 0.028mmol), continue to stir and react for 2 hours at room temperature, and then add Sodium hydroxide (1.12mg, 0.028mmol), and continue stirring reaction at room temperature for 1 hour, after filtering, evaporate the solvent to dryness with a rotary evaporator, and use dichloromethane (1mL)-n-hexane (10mL) mixed solvent [volume ratio is 1 :10] for recrystallization. The colorless crystalline product obtained by recrystallization was filtered, washed 3-4 times with 10 mL of diethyl ether, and dried in vacuo to obtain a colorless solid product (25.4 mg, 0.011 mmol) with a yield ...
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