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CAS No. : | 304445-49-6 | MDL No. : | MFCD00466241 |
Formula : | C8H6BrFO | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | VCTWSAITPPCBHI-UHFFFAOYSA-N |
M.W : | 217.04 | Pubchem ID : | 22831914 |
Synonyms : |
|
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302-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 |
---|---|---|
44% | With copper(ll) bromide; In ethyl acetate; at 60℃; for 12h; | A mixture of 1-(4-bromo-3-fluorophenyl)ethanone (1 g, 4.6 mmol), copper(II) bromide (2.1 g, 9.7 mmol) in EtOAc (50 mL) was stirred for 12 hours at 60 C. The mixture was allowed to cool down and filtered. The filtrate was concentrated. The residue was chromatographed (silica, ethyl acetate/petroleum ether) to give the desired compound as a yellow solid (600 mg, 44%). |
With phenyltrimethylammonium tribromide; In tetrahydrofuran; at 20℃; for 1h; | Step 3:; To a stirred solution of 1a3 (9.8 g, 45.3 mmol) in THF (90 mL) is added portionwise phenyltrimethylammonium tribromide (17.0 g, 45.3 mmol). The reaction mixture is stirred for 1 h at RT. Water is added, followed by EtOAc and the layers are separated. The organic layer is washed with water, brine, dried over MgS04, filtered and concentrated. The product is purified by flash chromatography using 100% hexanes to afford 1a4. | |
With copper(ll) bromide; In ethyl acetate; at 60℃; for 4h; | A solution of compound 4-1 (0.5 g, 2.3 mmol) and CuBr2 (1.13 g, 4.84 mmol) in EtOAc (5.0 mL) was stirred at 60 C for 4 hrs. After the reaction was completed, the mixture was cooled to rt and filtered. 20 mL of water was added to the filtrate and the resulting mixture was extracted with EtOAc (50 mL x 3). The combined organic layers were dried over anhydrous Na2S04 and concentrated in vacuo to give the title compound as a yellow solid (0.78 g). which was used for the next step without further purification. |
0.78 g | With copper(ll) bromide; In ethyl acetate; at 60℃; for 4h; | 10839] A solution of compound 4-1 (0.5 g, 2.3 mmol) and Cu13r2 (1.13 g, 4.84 mmol) in EtOAc (5.0 mE) was stirred at 60C. for 4 hrs. After the reaction was completed, the mixture was cooled tort and filtered. 20 mE of water was added to the filtrate and the resulting mixture was extracted with EtOAc (50 mEx3). The combined organic layers were dried over anhydrous Na2504 and concentrated in vacuo to give the title compound as a yellow solid (0.78 g), which was used for the next step without thrther purification. |
3.58 g | With phenyltrimethylammonium tribromide; In tetrahydrofuran; at 0 - 35℃; for 48h; | A) 2-bromo-1-(4-bromo-3-fluorophenyl)ethanone To a solution of 1-(4-bromo-3-fluorophenyl)ethanone (2.8 g) (obtained from 4-bromo-3-fluorobenzonitrile in the same manner as in Step B of Example 30) in tetrahydrofuran (150 mL) was added phenyltrimethylammonium tribromide (4.35 g) at 0C. The reaction mixture was stirred at room temperature for 2 days, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate) to give the title compound (3.58 g). 1H NMR (300 MHz, CDCl3) δ 4.33-4.42 (2H, m), 7.59-7.77 (3H, m). |
2.73 g | With bromine; acetic acid; at 20℃; for 3h; | 3-Fluoro-4-bromo-acetophenone (AA_117-1, 2.00 g, 9.22 mmol) was dissolved in acetic acid (15 mL), liquid bromine (0.47 mL, 9.22 mmol) was dripped. The reaction mixture was stirred at room temperature for 3 h. After the reaction was complete as detected by TLC, the solvent was removed by a rotary evaporator to deliver the target compound AA_117-2 (red brown solid, 2.73 g). The product was directly used for the next step without purification. 1H NMR (CDCl3, 400 MHz): δ 7.75-7.66 (m, 3H), 4.39 (s, 2H). |
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