Lithium pyridine formate complex, preparation method thereof and organic electroluminescent device
A picolinic acid, complex technology, applied in the direction of electric solid devices, lithium organic compounds, electrical components, etc., can solve the problems of numerical dispersion, difficult electron injection, difficult to control and so on
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Embodiment 1
[0079] 1. The preparation method of compound 5-methylpicolinate lithium
[0080] (1) Dissolve 1mol of 2-picoline in 10mol of benzene, put in ice bath, and slowly add 10g of anhydrous AlCl under stirring 3 , slowly add 1 mol of CH 3 Cl, slowly heated to 80°C, reacted for 12 hours, treated with concentrated hydrochloric acid and ice-water mixture, and distilled under reduced pressure to obtain 2,5-lutidine;
[0081](2) Dissolve the above-mentioned 2,5-lutidine in the aqueous solution (80%) of ethanol, add 1g KMnO 4 , After reacting for 2 hours, 5-picoline carboxylic acid was obtained, and then excessive metal Li was added to the reaction solution, under anhydrous and oxygen-free conditions, refluxed for 4 hours, the product was cooled and filtered, and 5-methylpicolin was obtained by column chromatography Lithium Picolinate.
[0082] The mass spectrum detection results of the compound are m / z: 143.06 (100.0%), 142.05 (8.2%), 144.06 (7.7%),
[0083] The hydrogen spectrum of t...
Embodiment 2
[0096] 1. The preparation method of compound 4-cyanopicolinate lithium
[0097] Prepared according to the same method as in the example, and the differences in reaction conditions are shown in Table 1 to obtain lithium 4-cyanopyridine carboxylate.
[0098] The mass spectrum detection results of the compound are m / z: 154.04 (100.0%), 153.03 (8.2%), 155.04 (7.7%),
[0099] The hydrogen spectrum of the compound is as image 3 As shown, the structure of the compound is as follows:
[0100]
[0101] 2. OLED devices containing the compound lithium 4-cyanopyridine carboxylate
[0102] The preparation method of the device of this embodiment is basically the same as that of Embodiment 1, the difference lies in the substance and thickness of each layer of vapor deposition;
[0103] The device structure of this embodiment is as figure 1 As shown, from bottom to top are:
[0104] ITO / 2-TNATA(15nm) / NPB(60nm) / TBPe:MADN (thickness 30nm, wherein MADN mass percentage is 2%) / Alq3(30nm) / ...
Embodiment 3
[0106] The preparation method of 1.6-trifluoromethylpicolinate lithium
[0107] Prepared according to the same method as in the example, and the differences in reaction conditions are shown in Table 1 to obtain lithium 6-trifluoromethylpicolinate.
[0108] The mass spectrum detection results of the compound are m / z: 197.03 (100.0%), 196.03 (8.2%), 198.03 (7.7%),
[0109] The hydrogen spectrum of the compound is as Figure 4 As shown, the structure of the compound is as follows:
[0110]
[0111] 2. OLED devices containing the compound 6-trifluoromethylpicolinate lithium
[0112] The preparation method of the device of this embodiment is basically the same as that of Embodiment 1, the difference lies in the substance and thickness of each layer of vapor deposition;
[0113] The device structure of this embodiment is as figure 1 As shown, from bottom to top are:
[0114] ITO / 2-TNATA(15nm) / NPB(60nm) / CBP:Ir(PPy) 3 (thickness 30nm, where Ir(PPy) 3 The mass percentage is 7...
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