9, 10-dipyrrolyl anthracene fluorescent compound as well as preparation method and application thereof
A fluorescent compound and compound technology, used in chemical instruments and methods, fluorescence/phosphorescence, luminescent materials, etc., can solve the synthesis and properties of asymmetric 9,10-thienyl anthracene compounds. No literature and patent reports have been reported, etc. problem, to achieve the effect of good cell staining function, simple synthesis and great application prospects
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[0050] The present invention provides a method for preparing the asymmetric 9,10-bisthienylanthracene aggregation-induced light-emitting compound described in the above scheme, comprising the following steps:
[0051] (i) when R is CN in formula I, the compound shown in formula I is 9-thienyl-10-(5-cyanothiophene) anthracene (TCTA), and preparation method comprises the following steps:
[0052] (1) Under a protective atmosphere, mix 9,10-dibromoanthracene, 2-thiopheneboronic acid, a palladium catalyst, a basic compound and a solvent for a Suzuki coupling reaction to obtain 9-thienyl-10-bromoanthracene; The molar ratio of 9,10-dibromoanthracene and 2-thiopheneboronic acid is 1:1~1.2;
[0053] (2) Under protective atmosphere, 9-thienyl-10-bromoanthracene, 2-cyano-5-boronic acid thiophene, palladium catalyst, basic compound and solvent are mixed for Suzuki coupling reaction to obtain 9-thienyl- 10-(5-cyanothiophene)anthracene; the molar ratio of 2-cyano-5-boronic acid thiophene ...
Embodiment 1
[0094] Preparation of 9-thienyl-10-(5-thienylcyano)anthracene (TCTA):
[0095] (1) Preparation of 9-thienyl-10-bromoanthracene:
[0096] Under nitrogen protection, 9,10-dibromoanthracene (3.36g, 10mmol) and Pd(PPh 3 ) 4 (10mol%) was dissolved in 80.0mLTHF, after stirring for 30min, 2-thiopheneboronic acid (2.10 g, 10.0mmol) was added and the concentration was 5.0equiv.Na 2 CO 3 Solution 60mL, heated to reflux for 12 h, stopped the reaction, cooled to room temperature. The solvent was removed by rotary evaporation, extracted with dichloromethane, the organic phases were combined, and dried over anhydrous magnesium sulfate. After suction filtration, the filtrate was rotary evaporated to remove the solvent, and separated by column chromatography using petroleum ether as the eluent to obtain a white solid (2.80 g, 6.6 mmol), yield: 66%.
[0097] (2) Preparation of 9-thienyl-10-(5-cyanothiophene) anthracene:
[0098] Under nitrogen protection, 9-thienyl-10-bromoanthracene (0...
Embodiment 2
[0101] Preparation of 9-thienyl-10-(5-hydroxythiophene)anthracene (THTA):
[0102] (1) Preparation of 9-thienyl-10-bromoanthracene:
[0103] Under nitrogen protection, 9,10-dibromoanthracene (3.36g, 10mmol) and Pd(PPh 3 ) 4 (10mol%) was dissolved in 80.0mLTHF, after stirring for 30min, 2-thiopheneboronic acid (2.10 g, 10.0mmol) was added and the concentration was 5.0equiv.Na 2 CO 3 Solution 60mL, heated to reflux for 12 h, stopped the reaction, cooled to room temperature. The solvent was removed by rotary evaporation, extracted with dichloromethane, the organic phases were combined, and dried over anhydrous magnesium sulfate. After suction filtration, the filtrate was rotary evaporated to remove the solvent, and separated by column chromatography using petroleum ether as the eluent to obtain a white solid (2.80 g, 6.6 mmol), yield: 66%.
[0104] (2) Preparation of 9-thienyl-10-(5-formylthiophene)anthracene:
[0105] Under nitrogen protection, 9-thienyl-10-bromoanthracen...
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