Serial oligomer with phenanthrene as constructional unit and its preparation method
An oligomer, a series of technologies, applied in a series of oligomers and their preparation fields, can solve the problems that hinder the application of organic thin film transistors, poor stability, etc.
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Embodiment 1
[0024] Embodiment 1: the synthesis of 2,7-dibromo-9,10-dihydrophenanthrene
[0025] at 5×10 5 Under the protection of Pa argon, add 3.64g of 9,10-dihydrophenanthrene to a 100ml three-necked flask, add 30ml of chloroform that has been dried with calcium hydride, 0.1g of anhydrous ferric chloride, and dissolve 2ml of liquid bromine Disperse in 10ml of chloroform, drop it into the three-necked flask within 30 minutes under ice bath conditions, stir and react at this temperature for 2 hours, remove the ice bath, continue stirring for 1 hour at room temperature, end the reaction, add saturated Sodium bisulfite aqueous solution 20ml, extract the organic phase, repeat twice, extract the aqueous layer with 20ml dichloromethane three times, combine the organic phase, wash the organic phase with 50ml saturated brine continuously for three times, and dry the organic phase with anhydrous magnesium sulfate , and the solvent was removed by rotary evaporation, and the obtained crude product...
Embodiment 2
[0026] Embodiment 2: the synthesis of 2-iodo-9,10-dihydrophenanthrene
[0027] Add 18g of 9,10-dihydrophenanthrene, 1.5ml of concentrated sulfuric acid, 100ml of glacial acetic acid, and 20ml of water into a 500ml three-necked flask, heat to 80°C and stir for 0.5 hours, then add 4.56g of periodic acid and 10.2g of ground iodine , the mixture was stirred at 80°C for 12 hours, the reaction was terminated, cooled to room temperature, 120ml of saturated aqueous sodium bisulfite solution was added, and the organic phase was obtained by extraction, which was repeated twice, and the aqueous layer was extracted three times with 120ml of dichloromethane. Combine the organic phases, wash the organic phases with 200ml of saturated brine continuously for three times, dry the organic phases with anhydrous magnesium sulfate, remove the solvent by rotary evaporation, separate and purify the obtained crude product by column chromatography, use petroleum ether as the eluent, and obtain 22.62g ...
Embodiment 3
[0028] Embodiment 3: the synthesis of 2,7-dibromophenanthrene
[0029]In a 500ml three-necked flask, add 2.7g of 2,7-dibromo-9,10-dihydrophenanthrene, 1.88g of bromosuccinimide (NBS), 0.23g of benzoyl peroxide (BPO), 200ml Carbon tetrachloride dried by calcium hydride, heated to reflux, stirred for 0.5 hours, stopped heating, cooled to room temperature, added 20ml of glacial acetic acid and 21g of potassium acetate, heated to reflux, stirred for 0.5 hours, stopped heating, cooled to room temperature, Continuously wash twice with 100ml water, then wash twice with 50ml 5% sodium carbonate aqueous solution, wash twice with 50ml saturated brine, dry the organic phase over anhydrous magnesium sulfate, remove the solvent by rotary evaporation, and use three The mixture of methyl chloride and petroleum ether was recrystallized to obtain 2.58 g of 2,7-dibromophenanthrene as white needle crystals with a yield of 95%.
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