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CAS No. : | 23449-08-3 | MDL No. : | MFCD00194632 |
Formula : | C21H14BrN3 | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | AYHGAQGOMUQMTR-UHFFFAOYSA-N |
M.W : | 388.26 | Pubchem ID : | 1728672 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | |
Hazard Statements: | H302-H315-H319-H335 | Packing Group: | |
GHS Pictogram: |
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* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
70% | With tris-(dibenzylideneacetone)dipalladium(0); triphenylphosphine; sodium t-butanolate; In tetrahydrofuran; toluene;Reflux; | triphenylen-2-ylboronic acid (5.4g, 20mmol) was dissolved in a THF 2-(4-bromophenyl)-4,6-diphenyl-1,3,5-triazine (7.8g, 20mmol), Pd2(dba)3 (0.9g, 1mmol), PPh3 (0.5g, 2mmol), followed by the addition of NaOt-Bu (5.8g, 60mmol), toluene (210 mL), stirred and refluxed. When the reaction is complete, the organic layer was dried over MgSO4, and extracted with water and ether and recrystallized silicagel column and the resulting organic compound and then concentrated and compound 5-6 was obtained 7.5g (70% yield). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
90% | With potassium phosphate; copper(l) iodide; (S,S)-1,2-diaminocyclohexane; In toluene; at 100℃;Inert atmosphere; | Compound 1 (0.60 g, 2.12 mmol), compound 2 (0.9 g, 2.32 mmol),tripotassium phosphate (0.89 g, 4.19 mmol), copper iodide (8 mg,0.04 mmol), and trans-1,2-diaminocyclohexane (0.21 g, 1.48 mmol)were dissolved in distilled toluene (40 mL), and the reaction mixture was refluxed at 100 C in N2 for 12 h. There after, the reaction mixturewas cooled to 25 C and filtered through Celite. It was concentrated under vacuum. The residue was purified by silica gel column chromatography using dichloromethane (DCM)/hexane (1:5 v/v) as the eluent to give a pure compound 3, which was a white-green solid (1.13 g);yield 90%. mp 255.6 C. IR (KBr, cm-1) ν: 2957, 1604, 1516, 1452,1370, 1219, 838, 772, 692. 1H NMR (CDCl3, 500 MHz, ppm): δ9.02-9.01 (2H, d, J=8.5 Hz), 8.82-8.80 (4H, dd, J=8.3, 1.5 Hz), 8.43(1H, s), 8.20-8.19 (1H, d, J=7.6 Hz), 7.85-7.84 (1H, d, J=7.7 Hz),7.83-7.81 (2H, dd, J=6.7, 1.8 Hz), 7.62 (1H, s), 7.61-7.60 (1H, t,J=1.7 Hz), 7.60-7.58 (3H, d, J=7.3 Hz), 7.57-7.56 (1H, t,J=1.7 Hz), 7.54-7.53 (2H, d, J=8.3 Hz), 7.44-7.40 (2H, m),7.38-7.35 (1H, td, J=7.5, 1.1 Hz), 7.34-7.31 (1H, t, J=7.5 Hz),7.29-7.26 (1H, td, J=7.4, 1.1 Hz), 1.53 (6H, s). 13C NMR (CDCl3,125 MHz, ppm): δ 170.91, 153.36, 153.31, 141.71, 140.86, 140.76,139.56, 136.10, 134.94, 132.80, 132.67, 130.70, 129.01, 128.70,127.07, 126.82, 126.40, 125.81, 124.01, 123.32, 122.56, 120.43,120.26, 119.41, 111.41, 109.92, 104.07, 46.81, 27.94; Uv-Vis (CHCl3) λ max/nm (ε/105 mol-1 dm3 cm-1): 362 (0.24); Found: [M+H]+590.2468; molecular formula C42H30N4 requires [M+H]+ 590.2470. |
With potassium tert-butylate; tri tert-butylphosphoniumtetrafluoroborate; In toluene; for 24h;Inert atmosphere; Reflux; | Added to the reaction bottle 0.1 μM intermediate 1, 0.1 μM intermediate 2, 20g tert-butanolate, 5g arrowhead three uncles acetate butyl phosphine tetrafluoroborate salts and toluene (1000 ml), under the protection of nitrogen heating reflux for 24 hours, cooling, removing the toluene, adding dichloromethane, washing, drying, the crude product of column, then methylene chloride and ethanol to recrystallize the purified product, compound 5. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
77% | With copper(l) iodide; 1,10-Phenanthroline; potassium hydroxide; In 5,5-dimethyl-1,3-cyclohexadiene; for 4.0h;Inert atmosphere; Reflux; | In a nitrogen atmosphereThe compound of formula IA (10 g, 50 mmol) and the compound of formula IB (19 g, 50 mmol)Was added to 250 ml of xylene and potassium hydroxide (5.6 g, 99 mmol), 1,10-phenanthroline (10 g, 19 mmol) was added with stirring.Then, by heating, copper iodide (2.8 g, 15 mmol) was slowly added under reflux. After the reaction was completed for about 4 hours, the reaction was terminated. After completion of the reaction, the temperature was lowered to room temperature, the salt was filtered through a filter, and the organic layer was distilled. Thereafter, the distillate was extracted twice with chloroform and water, and the organic layer was distilled off under reduced pressure Recrystallization with ethanol gave Intermediate 1 (19 g, 77percent). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
85% | With tris-(dibenzylideneacetone)dipalladium(0); tri-tert-butyl phosphine; sodium t-butanolate; In 1,4-dioxane; at 110℃; for 12h;Inert atmosphere; | Specific preparation process: 100ml under nitrogenTo the 1,4-dioxane solvent was added <strong>[3469-20-3]2,3-diphenylindole</strong> (1.70 g, 10.0 mmol)And 4-bromotriphenyltriazine (4.27g, 11.0mmol),Tris (dibenzylideneacetone) dipalladium (0.58 g, 0.5 mmol) and tri-tert-butyl phosphorus (15%, 0.15 mmol) were stirred at 110 C for 12 hours.After the reaction was cooled to room temperature, the mixture was filtered through a silica gel funnel, and the solution was concentrated under reduced pressure.The final product (4.90 g, 8.5 mmol) was obtained in a yield of 85%. |
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