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CAS No. : | 1072-97-5 | MDL No. : | MFCD00006323 |
Formula : | C5H5BrN2 | Boiling Point : | - |
Linear Structure Formula : | C5H3N(NH2)Br | InChI Key : | WGOLHUGPTDEKCF-UHFFFAOYSA-N |
M.W : | 173.01 | Pubchem ID : | 70622 |
Synonyms : |
|
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 |
---|---|---|
66% | With bis-triphenylphosphine-palladium(II) chloride In toluene at 130℃; for 16 h; Inert atmosphere | 5-Bromo-2-iodopyrimidine (10 g, 35.1 mmol) and tributyl(1-ethoxyethenyl)- stannane (15.85 g, 43.88 mmol) were dissolved in anhydrous toluene (500 mL) and purged with nitrogen for 10 minutes. Dichlorobis(triphenylphosphine)palladium(II) (1.23 g, 1.76 mmol) was added and the mixture was stirred at 130°C for 16 h. The reaction mixture was cooled to room temperature and water (29 mL) was added, followed by 6MHC1 (106 mL), then the mixture was stirred vigorously at room temperature for 4 h. The solvent was removed in vacuo and the pH of the mixture was adjusted to pH 7 by the addition of saturated aqueous sodium hydrogencarbonate solution (500 mL). The mixture was extracted with ethyl acetate (3 x 350 mL). The combined organic extracts were dried over magnesium sulfate, filtered and concentrated in vacuo. The crude material waspurified on silica gel, eluting with 20-100percent ethyl acetate in heptane, to afford the title compound (2.99 g, 66 percent) as a gold-coloured solid. LCMS m/z 20 1/203. |
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