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CAS No. : | 433939-27-6 | MDL No. : | MFCD07783710 |
Formula : | C6H4BrFO | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | JCPJGUPQZDEZQH-UHFFFAOYSA-N |
M.W : | 191.00 | Pubchem ID : | 21904636 |
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: |
* 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 |
---|---|---|
77% | With potassium carbonate; In acetonitrile; at 85℃; for 1h; | Example 15. Synthesis of 1-546-1. Into a 50-mL round-bottom flask, was placed <strong>[55876-84-1]methyl 5-(bromomethyl)picolinate</strong> (500 mg, 2.17 mmol, 1.00 equiv), 3-bromo-5-fluorophenol (440 mg, 2.30 mmol, 1.06 equiv), CH3CN (6 mL), and potassium carbonate (900 mg, 6.52 mmol, 3.00 equiv). The resulting solution was stirred for 60 min at 85°C. The mixture was concentrated under vacuum and the residue was diluted with 20 mL of H20. The resulting solution was extracted with 3x20 mL of ethyl acetate and the organic layers combined and dried over anhydrous sodium sulfate. The solids were filtered out. The resulting mixture was concentrated under vacuum. This resulted in 0.62 g (77percent) of methyl 5-((3-bromo-5- fluorophenoxy)methyl)picolinate as a yellow solid.LC-MS: ( + |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
71% | With potassium carbonate; In acetone; at 60℃; for 16h; | A solution of <strong>[19047-31-5]2-chloro-N-cyclopropylacetamide</strong> (2.8 g, 20.9 mmol), 3-bromo- 5-fluorophenol (4.0 g, 20.9 mmol) and K2CO3 (4.3 g, 31.4 mmol) in 40 mL of acetone was heated at 60 C for 16 h. The mixture was filtered and concentrated to give a residue, which was purified by column chromatography (PE/EA, 3/1) to give the title compound (4.3 g, 71%) as a yellow solid, m/e 288 (M+H)+. |
71% | With potassium carbonate; In acetone; at 60℃; for 16h; | Example 84 2-(3-Bromo-5-fluorophenoxy)-N-cyclopropylacetamide A solution of <strong>[19047-31-5]2-chloro-N-cyclopropylacetamide</strong> (2.8 g, 20.9 mmol), 3-bromo-5- fluorophenol (4.0 g, 20.9 mmol) and K2CO3 (4.3 g, 31.4 mmol) in 40 mL of acetone was heated at 60 C for 16 h. The mixture was filtered and concentrated to give a residue, which was purified by column chromatography (PE/EA, 3/1) to give the title compound (4.3 g, 71%) as a yellow solid, m/e 288 (M+H)+. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
38% | With sodium hydroxide; In water; at 120℃; for 120h; | To 3-bromo-5-fluoro-phenol (9.0 g, 47 mmol), and 1-chloro-2-methyl-propan-2-ol (5.116 g, 47.12 mmol), aqueous sodium hydroxide (37.69 g, 94.24 mmol) was added and the reaction mixture was heated at 120° C. for 5 days in a pressure vessel. The reaction was cooled and then extracted three times with ethyl acetate. The combined organic layer was dried over sodium sulfate, filtered, and the solvent was evaporated under reduced pressure. The crude product was purified on 220 g of silica gel utilizing a gradient of 0 to 10percent ethyl acetate in dichloromethane. The impure product was repurified on 220 g of gold silica gel utilizing a gradient of 0 to 10percent ethyl acetate in dichloromethane to yield 1-(3-bromo-5-fluoro-phenoxy)-2-methyl-propan-2-ol (4.75 g, 18.0 mmol, 38percent). ESI-MS m/z calc. 262.00046. found 263.0 (M+1)+. Retention time: 1.57 minutes (3 min run). |
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