Benzofluorene compound, material for light-emitting layer using same, organic electroluminescent element, display device, and lighting device
An organic electric field and compound technology, which is applied in the field of benzofluorene compounds, can solve problems such as unreported properties, and achieve the effect of improving properties
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[0272]
[0273] Hereinafter, the formula (1-1-11), formula (1-2-11), formula (1-1-1), formula (1-2-1) and formula (1-1-46) represent The synthesis example of the compound will be described.
Synthetic example 1
[0274] [Synthesis Example 1] Synthesis of Compound (1-1-11)
[0275] [chem 45]
[0276]
[0277]
[0278] Under nitrogen atmosphere, 1-naphthylboronic acid (38.0g), 2-bromo-5-chlorobenzoic acid methyl ester (50.0g), Pd(PPh 3 ) 4 (2.3g), potassium phosphate (85.0g), toluene (500ml), 2-propanol (150ml) and water (50ml) were stirred at reflux temperature for 2 hours. After cooling the reaction liquid to room temperature, water was added and liquid-separated, and the solvent was distilled off under reduced pressure. The obtained oily substance was purified by silica gel column chromatography (developing solution: toluene / heptane mixed solvent). At this time, referring to the method described in "Introduction to Organic Chemistry Experiments (1) - Substance Treatment and Separation and Purification -" published by Chemical Doujin Co., Ltd., page 94, slowly increase the ratio of toluene in the developing solution to make The target substance is dissolved. The eluate was di...
Synthetic example 2
[0291] [Synthesis Example 2] Synthesis of Compound (1-2-11)
[0292] [chem 46]
[0293]
[0294]
[0295] Under nitrogen atmosphere, N-phenylnaphthalene-1-amine (1.1g), 9-chloro-5-iodo-7,7-dimethyl-7H-benzo[c]fluorene (2.0g) were added A flask of dichlorobis(tri-o-tolylphosphine)palladium(II) (0.2g), sodium tert-butoxide (0.7g) and 1,2,4-trimethylbenzene (20ml) was stirred at 140°C 12 hours. After cooling the reaction liquid to room temperature, water and ethyl acetate were added and liquid-separated. After the solvent was distilled off under reduced pressure, it was purified by silica gel chromatography (developing solution: toluene / heptane / ethyl acetate=9 / 90 / 1 (volume ratio)). After distilling off the solvent under reduced pressure, the obtained solid was washed with heptane to obtain 9-chloro-7,7-dimethyl-N-(naphthalene-1-yl)-N-phenyl-7H- Benzo[c]fluoren-5-amine (1.0 g).
[0296]
[0297] Under nitrogen atmosphere, N-phenyl-4-(trimethylsilyl)aniline (0.53g), 9-c...
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