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CAS No. : | 244205-40-1 | MDL No. : | MFCD01114672 |
Formula : | C6H6BBrO2 | Boiling Point : | - |
Linear Structure Formula : | BrC6H4B(OH)2 | InChI Key : | PLVCYMZAEQRYHJ-UHFFFAOYSA-N |
M.W : | 200.83 | Pubchem ID : | 2773294 |
Synonyms : |
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Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H315-H319-H335 | Packing Group: | N/A |
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 |
---|---|---|
73.68% | With tetrakis(triphenylphosphine) palladium(0); potassium carbonate; In ethanol; water; toluene; for 6h;Inert atmosphere; Reflux; | In the 1L three bottles,9-bromo-phenanthroline (51.82 g, 0.20 mol) was added,O-bromobenzeneboronic acid (42.18 g, 0.21 mol)Potassium carbonate (55.2 g, 0.40 mol),165.6 g of water,Pd (PPh3) 4 (1.156 g, 1.0 mmol),Toluene (300 mL),Anhydrous ethanol (100 mL),N2 protection,Heating up to reflux,Insulation reaction 6 hours,Stop reaction, cool to 25 ,The organic phase was washed and neutralized. The organic phase was decompressed to remove the solvent. The solvent was purified by pure toluene column chromatography, toluene, ethanol recrystallization,To give intermediate 1-1 (yield 73.68percent). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
80% | With tetrakis(triphenylphosphine) palladium(0); sodium carbonate; In ethanol; water; toluene; for 18h;Reflux; | 4.00 g (17.1 mmol, 1.0 equiv.) of Intermediate b1, 4.12 g (20.51 mmol, 1.2 equiv.) of (2-bromophenyl)boronic acid, 1.38 g (1.20 mmol, 0.07 equiv.) of tetrakis(triphenylphosphine)palladium(0), and 4.53 g (42.72 mmol, 2.5 equiv.) of sodium carbonate were mixed with a solvent (0.6 M) in which toluene, ethanol, and distilled water (H2O) were mixed at a ratio of 3:1:1, and the resulting mixture was refluxed for 18 hours. The mixture obtained therefrom was cooled to room temperature, and a precipitate was filtered therefrom to obtain a solid. The obtained solid was washed with EA/H2O and purified by column chromatography (while increasing a rate of EA/Hex to between 5% and 10%) to obtain 4.24 g (yield: 80%) of Intermediate B1. The obtained product was identified by Mass and HPLC analysis. HRMS (MALDI) calcd for C17H12BrN: m/z 309.0153, Found: 309.0154. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
89% | With tetrakis(triphenylphosphine) palladium(0); potassium carbonate; In tetrahydrofuran; for 24h;Inert atmosphere; Reflux; | Pd(PPh3)4 (244 mg, 0.211 mmol, 0.05 equiv.), was charged to pressure tube contained <strong>[13534-90-2]3,4-dibromopyridine</strong> (1 g, 4.22 mmol, 1 equiv.), o-bromophenylboronic acid (848 mg, 4.22 mmol, 1 equiv.) under argon. The tube was backfilled with argon several times. The degassed THF (35 mL), 1M aqueous K2CO3 (25 mL) and 10% aqueous KOH (5 drops) was added under argon. The reaction mixture was backfilled with argon several times, then refluxed for 24 h. After cooling, the reaction mixture was diluted with dichloromethane (60 mL), and the resulting mixture was filtered through a pad of Celite, which was washed three times with dichloromethane (40 mL). The filtrate was concentrated in vacuo. The crude product was purified by flash chromatography (silica gel; hexane/ ethyl acetate, 5:1) to yield 3 (1.176 g, 89%) as colorless oil. 1H NMR (500 MHz, Chloroform-d) delta 8.84 (s, 1H), 8.59 (d, J = 4.9 Hz, 1H), 7.68 (dd, J = 8.1, 1.2 Hz, 1H), 7.44 - 7.37 (m, 1H), 7.30 (td, J = 7.8, 1.8 Hz, 1H), 7.22 - 7.17 (m, 2H); 13C NMR (126 MHz, Chloroform-d) delta 152.20, 149.49, 148.14, 139.33, 132.93, 130.25, 130.19, 127.42, 125.64, 122.20, 121.97. |
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