Application of pyridine tetrazole tetranuclear copper [I] complex in stimulus-responsive luminescent color-changing material
A pyridine tetrazolium and stimuli-response technology, which is applied in the direction of luminescent materials, color-changing fluorescent materials, copper organic compounds, etc., can solve the problem of few luminescent and color-changing materials
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[0026] The preparation mechanism of Method 1 is as follows:
[0027]
[0028]The second method of preparing pyridine tetrazolium tetranuclear copper [I] complex stimuli-responsive luminescent color-changing material:
[0029] Under argon atmosphere, copper perchlorate hexahydrate [Cu[ClO] with a molar ratio of 1:5-10:2:1 4 ] 2 ·6H 2 O], excess copper powder, N, N-bis[diphenylphosphoryl] amine [abbreviated dppa], 5-[2-pyridyl] tetrazole [abbreviated pytzH] in acetonitrile-dichloromethane mixed solvent [volume The ratio is 1:2] and stirred at room temperature for 2-4 hours, then added sodium hydroxide in an equimolar amount to the 5-[2-pyridyl]tetrazolium ligand to the reaction solution, and continued to stir and react at room temperature for 1 -2 hours, after filtering, use a rotary evaporator to evaporate the solvent to dryness under reduced pressure, use N,N-dimethylformamide [abbreviated as DMF]-ether mixed solvent [volume ratio of 1:10] for recrystallization, and filt...
Embodiment 1
[0039] Under an argon atmosphere, [Cu[CH 3 CN] 4 ][ClO 4 ] (29.5mg, 0.090mmol), N,N-bis[diphenylphosphoryl]amide (34.7mg, 0.090mmol) and 5-[2-pyridyl]tetrazolium (6.6mg, 0.045mmol) in 10mL Stir and react at room temperature in dichloromethane for 3 hours, then add sodium hydroxide (1.8mg, 0.045mmol) to the reaction solution, continue to stir and react at room temperature for 1 hour, then evaporate the solvent to dryness under reduced pressure with a rotary evaporator, and use N , N-dimethylformamide (1mL) - diethyl ether (10mL) mixed solvent [volume ratio 1:10] for recrystallization. The pale yellow crystalline product obtained by recrystallization was filtered, washed 3-4 times with 10 mL of ether, and dried in vacuo to obtain a pale yellow solid product (41.2 mg, 0.018 mmol), with a yield of 80%.
[0040] Elemental analysis calculated value (C 108 h 92 Cl 2 Cu 4 N 14 o 8 P 8 ) as (%): C 56.72, H 4.05, N 8.57; Found: C 56.75, H 4.07, N 8.54.
[0041] X-ray single c...
Embodiment 2
[0044] Under argon atmosphere, copper perchlorate hexahydrate [Cu[ClO 4 ] 2 ·6H 2 O] (18.5mg, 0.050mmol) and excess copper powder (21.6mg, 0.340mmol) were stirred in 5mL acetonitrile for 30 minutes at room temperature, and then N,N-bis[diphenylphosphoryl]amine (38.5mg, 0.100 mmol) in 10 mL of dichloromethane solution, continue to stir and react for 1 hour, add 5-[2-pyridyl]tetrazolium ligand (7.4mg, 0.050mmol), continue to stir and react for 2 hours at room temperature, and then add to the reaction solution Sodium hydroxide (2.0mg, 0.050mmol) was added, and the reaction was continued to stir at room temperature for 1 hour. After filtration, the solvent was evaporated to dryness under reduced pressure with a rotary evaporator, and N,N-dimethylformamide (1mL)-diethyl ether ( 10mL) mixed solvent [volume ratio 1:10] for recrystallization. The pale yellow crystalline product obtained by recrystallization was filtered, washed 3-4 times with 10 mL of ether, and dried in vacuo to o...
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