| 67% |
With tetrakis(triphenylphosphine) palladium(0); potassium carbonate In tetrahydrofuran; water; toluene for 12h; Inert atmosphere; Reflux; |
11 Synthesis Example 11: Synthesis of Compound A17
15.00 g (37.66 mmol) of 3-bromo-N-meta-biphenylcarbazole, 16.77 g (37.66 mmol) of 3-boronic ester-N-biphenyl carbazole, 200 mL of a mixture of tetrahydrofuran (THF) and toluene (1:1), and 100 mL of an aqueous solution of 2 M potassium carbonate were mixed in a 500-mL round-bottom flask equipped with a stirrer in a nitrogen atmosphere, and 2.18 g (1.88 mmol) of tetrakis(triphenylphosphine)palladium(0) was added thereto, and heated under reflux in a nitrogen atmosphere for about 12 hours. After completion of the reaction, the reaction product was added to methanol to obtain a solid by filtering. This solid was thoroughly washed with water and methanol, and then dried. The resulting product was dissolved in 500 mL of chlorobenzene by heating, followed by filtration using silica gel and removing the solvent. The resulting product was dissolved in 400 mL of toluene by heating, followed by recrystallization to obtain Compound A17 (16.07 g, Yield: 67%). calcd. C48H32N2: C, 90.54; H, 5.07; N, 4.40; found: C, 90.71; H, 5.01; N, 4.27 |
| 67% |
With tetrakis(triphenylphosphine) palladium(0); potassium carbonate In tetrahydrofuran; water; toluene for 12h; Inert atmosphere; Reflux; |
18 Synthesis of Compound A17
Nitrogen atmosphere equipped with a stirrer 500 mL round bottom flask, 3-bromo-meta -N- biphenyl-carbazole 15.00 g (37.66mmol), 3- Bono Nick ester -N- biphenyl-carbazole 16.77 g (37.66 mmol) and tetrahydrofuran: toluene (1: 1) 200 mL andAfter mixing the aqueous solution of potassium carbonate 2M- 100mL, tetrakistriphenylphosphine palladium (0) 2.18 g (1.88mmol) and the mixture a stream of nitrogenUnder the mixture was heated under reflux for 12 hours. After completion of the reaction the reaction was poured into a methanol, the solid was filtered and then, therefromThe solid obtained was thoroughly washed with water and methanol and dried. The results obtained therefrom in 500mL of chloro benzeneThe solid dissolved and then the solution was purified by silica gel filter, and then dissolved by the solvent is removed completely, and heated in 400mL of toluene and thenRecrystallization to give the compound A17 16.07 g (yield 67%). |
| 67% |
With tetrakis(triphenylphosphine) palladium(0); potassium carbonate In tetrahydrofuran; toluene for 12h; Inert atmosphere; Reflux; |
11 synthesis of compound A17
a stirring under a nitrogenatmosphere 500 ml round bottom flask 3-bromo-n-metabiphenylcarbazole 15.00g (37.66 mmol ), 3-boronicester-n-biphenyl carbazole 16.77 g (37.66 mmol ) andtetrahydrofuran: toluene (1: 200 ml and 2M-potassium carbonate solution aftermixing a 100 ml, tetrakisazo methylphenylphosphinic triphenylimidazolespalladium 0. 88mmol -2.18 g (1 ) in the presence of nitrogen air stream in awas heated to reflux for a period of 12 hours. After the termination of thereaction the reaction filtered and then poured into methanol in the solidobtained therefrom, with water and methanol, and the solid is rinsed and driedsufficiently. The results obtained therefrom in 500 mL of chlorobenzenesolution of the dissolved solids then removed and the solvent completelyfilters and silica gel, 400 ml of toluene to be dissolved by heating thecompound a17 yielded16.07 g (yield 67%). |
| 67% |
With tetrakis(triphenylphosphine) palladium(0); potassium carbonate In tetrahydrofuran; toluene Inert atmosphere; Reflux; |
Synthesis of Compound B-43
Under a nitrogen atmosphere, to a 500 mL round bottom flask equipped with a stirrer was added 3-bromo-N-methabiphenylcarbazole 15.00 G (37.66 mmol), 16.77 g (37.66 mmol) of 3-bononic ester-N-biphenylcarbazole and 1: 1 of tetrahydrofuran: And 100 mL of a 2M potassium carbonate aqueous solution were mixed, and 2.18 g (1.88 mmol) of tetrakistriphenylphosphine palladium (0) was added thereto The mixture was heated under reflux for 12 hours under a stream of nitrogen. After completion of the reaction, the reaction product is poured into methanol to filter out the solid matter Well, the solids obtained therefrom were sufficiently washed with water and methanol and dried. The resulting product was dissolved in 500 mL of The solids were dissolved in chlorobenzene and the solution was then filtered through silica gel, the solvent was removed completely and heated to 400 mL of toluene , And then recrystallized to obtain 16.07 g (yield 67%) of the compound B-43. |
| 67% |
With tetrakis(triphenylphosphine) palladium(0); potassium carbonate In tetrahydrofuran; water; toluene for 12h; Inert atmosphere; Reflux; |
19 Synthesis of Compound B-136
15.00 g (37.66 mmol) of 3-bromo-N-metabiphenylcarbazole and 16.77 g (37.66 mmol) of 3-boronic ester-N-biphenyl carbazole were mixed with 200 mL of tetrahydrofuran and toluene (1:1) and 100 mL of a 2 M-potassium carbonate aqueous solution in a 500 mL round-bottomed flask equipped with an agitator under a nitrogen atmosphere, 2.18 g (1.88 mmol) of tetrakistriphenylphosphinepalladium (0) was added thereto, and the mixture was heated and refluxed under a nitrogen flow for 12 hours. When a reaction was complete, the reactant was poured into methanol, and a solid therefrom was filtered, sufficiently cleaned with water and methanol, and dried. The obtained resulting material was dissolved in 500 mL of chlorobenzene, the solution was silica-gel filtered, and a filtrate therefrom was heated and dissolved in 400 mL of toluene after completely removing the solvent and recrystallized to obtain Compound B-136 (16.07 g, yield of 67%). (0264) calcd. C48H32N2: C, 90.54; H, 5.07; N, 4.40; found: C, 90.71; H, 5.01; N, 4.27 |
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