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CAS No. : | 104197-13-9 | MDL No. : | MFCD00236213 |
Formula : | C6H3BrF2O | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | GPRPSJPFAAGLCA-UHFFFAOYSA-N |
M.W : | 208.99 | Pubchem ID : | 2736292 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | |
Hazard Statements: | 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 |
---|---|---|
68% | With potassium carbonate; In acetone; at 0 - 20℃; for 22h; | Intermediate 111 5-bromo-1,3-difluoro-2-methoxybenzene To a solution of intermediate 110 (15.0 g, 71.73 mmoles) in acetone (60 mll), potassium carbonate (29.75 g, 215.32 mmoles) was added at 0 C. followed by methyl iodide (22 ml, 358.86 mmoles) and stirred at RT for 22 h. The reaction mixture was concentrated, diluted with water and extracted with ethyl acetate. The organic layer was dried over sodium sulphate and concentrated under reduced pressure to afford the title compound as light yellow liquid (11 g, 68% yield). 1H-NMR (delta ppm, DMSO-D6, 400 MHz): delta 7.08 (d, J=7.8 Hz, 2H). |
With potassium carbonate; In acetone; at 0 - 60℃; | ii) 4-Bromo-2,6-difluorophenyl methyl ether Methyl iodide (17.11 g, 0.12 mol) was added at 0C to a well stirred suspension of 4-bromo-2,6-difluorophenol (21 g, 0.1 mol; see step (i) above) and K2CO3 (27.78 g, 0.2 mol) in dry acetone (150 mL). Stirring was continued at 6O0C overnight under a nitrogen atmosphere. The reaction mixture was filtered, the solvent was evaporated and the residue was purified by column chromatography over silica gel, using petroleum ether as eluent, to give 11.5 g of the sub-title compound as a colourless liquid. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With caesium carbonate; In N,N-dimethyl acetamide; at 80℃; for 3.0h; | 5-Bromo-1,3-difluoro-2-(3-methanesulfonyl-propoxy)-benzene A mixture of 4-bromo-2,6-difluoro-phenol (500 mg), <strong>[357913-53-2]methanesulfonic acid 3-methanesulfonyl-propyl ester</strong> (517 mg), and cesium carbonate (1.56 g) in N,N-dimethylacetamide (10 mL) is heated to 80 C. for 3 h. The reaction mixture diluted with water and extracted with ethyl acetate. The combined extracts are dried over Na2SO4 and concentrated in vacuo. The residue is chromatographed on silica gel (cyclohexane/ethyl acetate 100:0?80:20) to give the title compound. |
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