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With tetrakis(triphenylphosphine) palladium(0); sodium carbonate; In ethanol; water; toluene; for 2.0h;Inert atmosphere;
Under the protection of nitrogen gas to a three-necked flask of 250ml 4,4'- diphenylether hypo-3-boric acid 5.7g (22mmol), M37-220g (44mmol), tetrakis triphenylphosphine palladium 2g, 100ml toluene, ethyl alcohol 60ml, water 80ml and 16g of sodium carbonate is added, and the progress Circulating react for 2 hours. After the results gamcheuk and shown by TLC to stop the reaction when the complete reaction was cooled to room temperature fraction ( ) and washed with water and extract the award and merges the organic phase, dry, rotating dewatering (Spin Dry) through a yellow oil It gained the material.Column chromatography (dichloromethane / petroleum ether) to proceed to a white solid 13.0g was obtained to be 64% yield.
64%
With tetrakis(triphenylphosphine) palladium(0); sodium carbonate; In ethanol; water; toluene; for 2.0h;Inert atmosphere; Reflux;
In a 250 ml three-necked bottle under nitrogen protection,(22 mmol) of 4,4'-diphenyl ether diboric acid, 2 g of borate (22 mmol), M37-2 20 g (44 mmol), 2 g of tetrakis (triphenylphosphine palladium), 100 ml of toluene, 60 ml of ethanol, 16 g of sodium carbonate, , Reflux reaction for 2 hours, TLC showed complete reaction. The reaction was stopped, cooled to room temperature, partitioned, washed with water, extracted with water, and the organic phases were combined, dried and dried to give a yellow oil. Column chromatography (dichloromethane / petroleum ether) gave 13.0 g of a white solid in 64% yield.
With tetrakis(triphenylphosphine) palladium(0); sodium carbonate; In ethanol; water; toluene; for 2.0h;Inert atmosphere;
A 500ml three-necked flask equipped with a mechanical stirrer fitted under the protection of nitrogen gas4,4'-diphenylether hypo-boric acid 3-phenyl-carbazol--N-25.8g (100mmol),3-bromo-benzothiophene-51g (220mmol), tetrakistriphenylphosphinepalladium 3.5g, 150ml of toluene, ethyl alcohol 50ml, 100ml water and 53g of sodium carbonate for 2 hours dongan Circulating In response to the progress. TLC in gamcheuk and It presented the results to stop the reaction when the complete reaction and then cooled to room temperature, aliquots (Separated ), washed and extracted water with water, through the merging of the organic phase, dry, rotary dehydration (Spin dry) to obtain the oil-phase material as a yellow . a column chromatography (dichloromethane / petroleum ether), this 64% yield was obtained as a white solid 27.8g proceeds.
64%
With tetrakis(triphenylphosphine) palladium(0); sodium carbonate; In ethanol; water; toluene; for 2.0h;Inert atmosphere; Reflux;
To a 500 ml three-necked flask equipped with mechanical stirrer and nitrogen protection, 25.8 g (100 mmol) of 4,4'-diphenyl ether diboric acid, 3-boronic acid-N-phenylcarbazole, 51 g of 3-bromobenzothiophene (Toluene) palladium, 3.5 ml of toluene, 50 ml of ethanol, 53 ml of sodium carbonate and 100 ml of water were refluxed for 2 hours. TLC showed complete reaction. The reaction was stopped, cooled to room temperature, partitioned, washed with water, extracted with water, and the organic phases were combined, dried and dried to give a yellow oil. Column chromatography (dichloromethane / petroleum ether) gave 27.8 g of a white solid in 64% yield.