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CAS No. : | 446-48-0 | MDL No. : | MFCD00000324 |
Formula : | C7H6BrF | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | FFWQLZFIMNTUCZ-UHFFFAOYSA-N |
M.W : | 189.02 | Pubchem ID : | 67968 |
Synonyms : |
|
Signal Word: | Danger | Class: | 8 |
Precautionary Statements: | P261-P280-P305+P351+P338-P310 | UN#: | 3265 |
Hazard Statements: | H227-H314-H335 | Packing Group: | Ⅱ |
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 |
---|---|---|
109 g | With potassium carbonate; hydrazine hydrate In ethanol at 0℃; for 48 h; | With stirring, 190 g (1.0 mol) of 2-fluorobenzyl bromide were added to a mixture of 250 g (5.0 mol) of hydrazine hydrate and 137 g (1.0 mol) of potassium carbonate in 2 l of ethanol. The mixture was stirred at room temperature for 2 d and then concentrated under reduced pressure. The residue was extracted with diethyl ether. The organic phase was dried over sodium sulphate and concentrated. The crude product was purified by chromatography on silica gel. This gave 109 g (76percent of theory) of the target compound. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
23% | With copper(l) iodide; lithium methanolate; triphenylphosphine In N,N-dimethyl-formamide at 20℃; for 14 h; Inert atmosphere | 2-Fluorobenzyl bromide (3000 mg, 15 mmol), boronic acid pinacol ester (6000 mg, 24 mmol),CuI (320 mg, 1.5 mmol), LiOMe (1200 mg, 32 mmol), PPh3 (540 mg, 2 mmol) and DMF (50 mL) were placed in a 250 mL reaction flask and replaced with nitrogen three times and then reacted for 14 h at room temperature. The reaction solution was poured into 200 mL of water, and the CuI was removed by filtration and washed three times with EA. The filtrate was collected and separated, and the aqueous extracted with EA (150 mL×3). After concentrating the EA layer, the title compound 52b (980 mg, 23percent) |
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