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CAS No. : | 50548-45-3 | MDL No. : | MFCD00094238 |
Formula : | C12H7BrO | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | WUYYVOWEBMOELQ-UHFFFAOYSA-N |
M.W : | 247.09 | Pubchem ID : | 190542 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P280-P305+P351+P338 | UN#: | |
Hazard Statements: | H302 | Packing Group: | |
GHS Pictogram: |
* 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 |
---|---|---|
95% | With sodium hydride; In N,N-dimethyl-formamide; at 0 - 100℃; for 1.33333h; | General procedure: Compound A-2 (40.0 g, 132.7 mmol) was dissolved in distilled dimethylformamide (400 mL). It cooled to 0 ,Sodium hydride (3.5 g, 145.9 mmol) was slowly added dropwise thereto. The mixture was stirred for 20 minutes and then at 100 ° C for 1 hour. After completion of the reaction, the reaction mixture was cooled to room temperature,Ethanol (100 mL) was slowly added.The mixture was distilled under reduced pressure, and the resulting mixture was extracted with chloroform,And recrystallized from ethyl acetate to obtain Compound A-3 (30.3 g, yield 81percent). |
95% | With sodium hydride; In N,N-dimethyl-formamide; at 0 - 100℃; for 1.3h; | General procedure: Compound A-2 (40.0 g, 132.7 mmol) was dissolved in distilled dimethylformamide (400 mL)Respectively. It cooled to 0 , sodium hydride here(3.5 g, 145.9 mmol) was slowly added dropwise.Stir for 20 minutes and then stir at 100 for 1 hour. After the reaction was completed, the reaction mixture was cooled to room temperature, and ethanol (100 mL) was slowly added thereto. The mixture was vacuum distilled, and the resulting mixture was recrystallized from chloroform and ethyl acetate to obtain Compound A-3 (30.3 g, yield 81percent)It was obtained. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
100% | With (1,1'-bis(diphenylphosphino)ferrocene)palladium(II) dichloride; potassium acetate; In 1,4-dioxane; for 24h;Reflux; | 31.3 g (126.7 mM) of <strong>[50548-45-3]1-bromodibenzo[b,d]furan</strong>, (<strong>[50548-45-3]1-bromodibenzo[b,d]furan</strong>),190.0 g (190.0 mM) bis (pinacolato) diboron, 4.6 g (6.3 mM) PdCl2(dppf) 37.3 g (380.1 mM) of KOAc was dissolved in 300 mL of 1,4-dioxane and refluxed for 24 hours. After the reaction was completed, distilled water and DCM (dichloromethane) were added at room temperature. The organic layer was dried with MgSO 4 and the solvent was removed by a rotary evaporator. The reaction product was purified by column chromatography (DCM: Hex = 1: 3) and recrystallized from methanol to obtain the desired compound 1-5-3 37 g (quant.). |
98% | With palladium diacetate; calcium acetate; In N,N-dimethyl-formamide; at 80℃;Inert atmosphere; | 101g (410 mmol) of <strong>[50548-45-3]1-bromodibenzofuran</strong> was added to 500 ml flask under protectivegas, 273 g (1055 mmol) of bis (pinacolato) diborane (CAS 73183-34-3) wasdissolved in in 1500 ml dry DMF and degassed for 30 minutes. 121 g (1229 mmol) Calciumacetate and 8.4 g (37 mmol) palladium acetate are added subsequently, and thebatch was heated overnight at 80C . When the reaction was complete, themixture was diluted with 300 ml of toluene, and extracted with water. Thesolvent was removed in rotary evaporator, and the product was thenrecrystallized from heptane. Yield: 118 g (401mmol), 98% theory. |
70% | With (1,1'-bis(diphenylphosphino)ferrocene)palladium(II) dichloride; potassium acetate; In 1,4-dioxane; for 10h;Reflux; | 500ml round bottom flask reactor, <strong>[50548-45-3]1-bromodibenzofuran</strong>(20.0g, 0.081mmol), bis(pinacolato)diboron (26.7g, 0.105mol), [1,1'-bis(diphenylphosphino)ferrocene]palladium dichloride (1.3g, 0.002mol), potassium acetate (19.9g, 0.202mol), into a 1,4-dioxane 200ml were stirred for 10 hours under reflux after completion of the reaction was filtered a pad of celite. Filtrate was concentrated under a reduced pressure was separated and then the column was recrystallized from dichloromethane and heptane to give a intermediate 4-a> (17.0g, 70%). |
70% | With (1,1'-bis(diphenylphosphino)ferrocene)palladium(II) dichloride; potassium acetate; In 1,4-dioxane; for 10h;Reflux; | 500ml round bottom flask reactor1-Bromo-dibenzofuran (20.0g, 0.081mmol), Bis (pinacolato) diboron (26.7g, 0.105mol),[1,1'-bis (diphenylphosphino) ferrocene] palladium in a Dijk (1.3g, 0.002mol),Potassium acetate (19.9g,0.202mol), into a 1,4-dioxane 200ml were stirred for 10 hours under reflux. After the completion of the reaction was filtered a pad of Celite. femaleAfter concentration under reduced pressure they were separated by liquid column and recrystallized with dichloromethane-heptane to give a (17.0g, 70%). |
70% | With (1,1'-bis(diphenylphosphino)ferrocene)palladium(II) dichloride; potassium acetate; In 1,4-dioxane; for 10h;Reflux; | <strong>[50548-45-3]1-bromodibenzofuran</strong> (20.0 g, 0.081 mmol) was charged in a 500 ml round bottom flask reactor,Bis (pinacol) diboron (26.7 g, 0.105 mol)[1,1'-bis (diphenylphosphino) ferrocene] dichloropalladium (1.3 g, 0.002 mol)Potassium acetate (19.9 g, 0.202 mol), 200 ml of 1,4-dioxane and stirred under reflux for 10 hours.After the reaction was complete, the diatomaceous earth liner was filtered. The filtrate was concentrated under reduced pressure and then separated by column,And recrystallized from dichloromethane and heptane to obtain (17.0 g, 70%). |
70% | With (1,1'-bis(diphenylphosphino)ferrocene)palladium(II) dichloride; potassium acetate; In 1,4-dioxane; for 1h;Reflux; | In a 500-mL round-bottom flask reactor, <strong>[50548-45-3]1-bromodibenzofuran</strong> (20.0 g, 0.081 mmol), bis(pinacolato)diboron (26.7 g, 0.105 mol), [1,1?-bis(diphenylphosphino)ferrocene]dichloropalladium (1.3 g, 0.002 mol), potassium acetate (19.9 g, 0.202 mol), and 1,4-dioxane (200 ml) were stirred together for hrs under reflux. After completion of the reaction, filtration was performed through a celite pad. The filtrate was concentrated in a vacuum, purified by column chromatography, and recrystallized in dichloromethane and heptane to afford <Intermediate 4-a> (17.0 g, 70%). |
70% | With dichloro(1,1'-bis(diphenylphosphanyl)ferrocene)palladium(II)*CH2Cl2; potassium acetate; In 1,4-dioxane; for 10h;Reflux; | In a 500-mL round-bottom flask reactor, <strong>[50548-45-3]1-bromodibenzofuran</strong> (20.0 g, 81 mmol), bis(pinacolato)diboron (26.7 g, 105 mmol), [1,1?-bis(diphenylphosphino)ferrocene]dichloropalladium (1.3 g, 0.002 mol), potassium acetate (19.9 g, 202 mmol), and 1,4-dioxane (200 ml) were stirred together for 10 hrs under reflux. Concentration in a vacuum was followed by column chromatographic purification. Recrystallization in dichloromethane and heptane afforded (17.0 g, 70%). |
70% | With (1,1'-bis(diphenylphosphino)ferrocene)palladium(II) dichloride; potassium acetate; In 1,4-dioxane; for 10h;Reflux; | Intermediate 8-a was synthesized according to Scheme 60 below:<strong>[50548-45-3]1-bromodibenzofuran</strong> (20.0g, 0.081mmol), bis (pinacolato) diboron (26.7g, 0.105mol) in 500ml round bottom flask reactor,200 ml of [1,1'-bis (diphenylphosphino) ferrocene] dichloropalladium (1.3 g, 0.002 mol), potassium acetate (19.9 g, 0.202 mol) and 1,4-dioxane were added and stirred under reflux for 10 hours. . After the reaction was completed, the celite pad was filtered. The filtrate was concentrated under reduced pressure and column separatedRecrystallization from dichloromethane and heptane gave |
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