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With (1,1'-bis(diphenylphosphino)ferrocene)palladium(II) dichloride; sodium tetrahydroborate; N,N,N,N,-tetramethylethylenediamine; In tetrahydrofuran; at 25℃;Inert atmosphere;
General procedure: PdCl2(dppf), PdCl2(tbpf) and (A.caPhos)PdCl2. A mixture of the halogenated heterocycle (0.66 mmol) in anhydrous THF (13.2 mL) was degassed by bubbling argon for few minutes. Then, PdCl2(dppf) (27.0 mg, 0.033 mmol, 5.0 mol%), TMEDA (0.130 g, 1.12 mmol, 1.7 equiv) and finally NaBH4 (42.4 mg, 1.12 mmol, 1.7 equiv) were introduced in sequence. The mixture was stirred at room temperature under argon for the proper time and then worked up as described above.
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.
With tetrakis(triphenylphosphine) palladium(0); potassium carbonate; In water; toluene; for 12h;Reflux; Inert atmosphere;
9-phenyl-3,6-bis(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl) -9H-carbazole 10.0 g (20.19 mmol)9.47 g (44.42 mmol) of 3-bromobenzothiophene,12.28 g (88.85 mmol) of K2CO3, Pd (PPh3) 4 0.47 g (0.40 mmmol) 100 ml of toluene,Suspended in distilled water (50 ml), and stirred under reflux for 12 hours under a stream of nitrogen. After completion of the reaction, the reaction solution was extracted with dichloromethane, filtered through silica gel, and distilled under reduced pressure. Then, hexane: dichloromethane = 7: 3 (v / v)To obtain Compound 217.3 g (Yield: 71percent).
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