Spirofluorene organic laser material based on trifluoromethyl benzene functionalization, microcrystal preparation and application
A technology of trifluoromethylbenzene and trifluoromethylbenzene group, which is applied in the field of organic electroluminescence, can solve the problems of poor repeatability and interference, and achieves low ASE threshold, regular morphology and high yield Effect
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Embodiment 1
[0028] Synthesis of Example 1 Precursor 1, 2 and 3
[0029] The structures of precursors 1, 2 and 3 are shown below:
[0030]
[0031] The synthesis methods of precursors 1, 2 and 3 are the same. Here, the synthesis of precursor 1 is taken as an example. The specific synthesis route and steps are as follows:
[0032]
[0033] 2,7-Dibromospirofluorene (2.37g, 5mmol), bis-pinacol borate (3.04g, 12mmol), Pd(OAc) 2 (0.11g, 0.5mmol), dppf (0.55g, 1mmol), KOAc (1.47g, 15mmol) were placed in a 100mL two-necked round bottom flask, and the air in the flask was replaced with nitrogen three times. Add 1,4-dioxane (50 mL), heat to 90° C., and react for 6 hours. Add water to quench the reaction, extract with ethyl acetate, dry the organic layer with anhydrous sodium sulfate, remove the solvent by rotary evaporation, and separate by column chromatography to obtain precursor 1 (2.61 g, 92%).
Embodiment 2
[0034] Embodiment 2 Synthesis of trifluoromethylbenzene-based organic laser materials 1, 2 and 3 based on spirofluorene
[0035] Its structural formula is as follows:
[0036]
Embodiment 3
[0037] Example 3 The synthesis methods of spirofluorene-based trifluoromethylbenzene-based organic laser materials 1, 2 and 3 are the same. Here, the synthesis of spirofluorene-based trifluoromethylbenzene-based organic laser materials 1 is an example. The specific synthesis route and Proceed as follows:
[0038]
[0039] 3,5-bistrifluoromethylbromobenzene (0.64g, 2.2mmol), precursor 1 (0.57g, 1.0mmol), Pd(PPh 3 ) 4 (0.115g, 0.1mmol), placed in a 100mL two-necked round-bottomed flask and replaced the air in the bottle with nitrogen three times. Join K 2 CO 3 Solution (2M, 2.0 mL), toluene / tetrahydrofuran (1:1, 20 mL) which was bubbled with nitrogen for 2 hours in advance was added to the reaction system. Heat to 90, react for 24 hours. Add water to quench the reaction, extract with dichloromethane, dry the organic layer over anhydrous sodium sulfate, remove the solvent by rotary evaporation, and separate by column chromatography to obtain an organic laser material 1 ba...
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