Thermal activation delayed fluorescence material and application thereof
A technology of thermally activated delay and fluorescent materials, applied in the field of organic electroluminescent devices, can solve the problems of efficiency roll-off, severe, and insufficient stability of TADF materials, and achieve good photoelectric performance, good thermal stability and film-forming properties, The effect of novel structure
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[0045] The preparation of embodiment intermediate
[0046]
[0047] 1. Synthesis of Intermediate I
[0048] In the flask, add 5,8-dibromo-2,3-diphenylquinoxaline (10g, 22.7mmol), carbazole (3.4g, 20.3mmol), sodium tert-butoxide (3.3g, 34.3mmol), PD 2 (dba) 3 (0.15g), tri-tert-butylphosphine (0.1g) and 100mL anhydrous toluene, reflux reaction for 2 hours, add dilute hydrochloric acid to adjust to weakly acidic liquid separation, dry, concentrate, and the crude product is recrystallized from toluene to obtain 7.2g, the yield 60%. 1 H NMR (400MHz, CDCl 3)δ: 8.11-8.14(m, 2H), 8.04(d, J=7.2Hz, 1H), 7.82(d, J=7.6Hz, 1H), 7.61-7.63(m, 2H), 7.50-7.57(m ,4H),7.32-7.38(m,8H),7.20-7.24(m,2H).HRMS(ESI,m / z):[M+H] + 526.10.
[0049] 2. Synthesis of Intermediate II
[0050] In the flask, add intermediate I (7g, 13.3mmol), pinacolate (4.1g, 16.1mmol), potassium acetate (3.9g, 39.7mmol), Pd (PPh 3 ) 3 Cl 2 (0.07g), 70mL of anhydrous toluene, reflux reaction for 5 hours, cooled, p...
Embodiment 1
[0056] The synthesis of embodiment 1 compound 1
[0057]
[0058] Intermediate II (2.0g, 3.49mmol), 1,4-dibromobenzene (0.40g, 1.70mmol), potassium carbonate (0.70g, 5.09mmol), Pd(PPh 3 ) 4 (0.01g), then add toluene (10mL), ethanol (5mL) and deionized water (5mL), reflux reaction under nitrogen protection for 5 hours, liquid separation, concentration, crude product obtains 1.4g white product through column chromatography, productive rate is 86%. 1 HNMR (400MHz, CDCl 3 )δ: 8.11-8.14(m, 4H), 7.93(d, J=6.4Hz, 2H), 7.79(d, J=6.4Hz, 2H), 7.53-7.59(m, 12H), 7.47-7.49(m ,4H),7.30-7.37(m,16H),7.19-7.24(m,4H).HRMS(ESI,m / z):[M+H] + 969.35.
Embodiment 2
[0059] The synthesis of embodiment 2 compound 9
[0060]
[0061] Intermediate II (2g, 3.49mmol), 2,5-dibromopyridine (0.40g, 1.69mmol), potassium carbonate (0.70g, 5.06mmol), Pd(PPh 3 ) 4 (0.01g), then add toluene (10mL), ethanol (5mL) and deionized water (5mL), reflux reaction under nitrogen protection for 5 hours, liquid separation, concentration, crude product obtains 1.3g white product through column chromatography, productive rate is 80%. 1 HNMR (400MHz, CDCl 3 )δ: 9.43(d, J=2.0Hz, 1H), 8.07-8.14(m, 6H), 7.94(d, J=6.8Hz, 1H), 7.80-7.88(m, 3H), 7.54-7.59(m ,8H),7.47-7.49(m,4H),7.30-7.37(m,16H),7.19-7.24(m,4H).HRMS(ESI,m / z):[M+H] + 970.35.
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