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CAS No. : | 118289-16-0 | MDL No. : | MFCD04039313 |
Formula : | C6H6BrNO | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | IQNUGAFIKDRYRP-UHFFFAOYSA-N |
M.W : | 188.02 | Pubchem ID : | 14512957 |
Synonyms : |
|
Chemical Name : | 2-Bromopyridine-4-methanol |
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 |
---|---|---|
With manganese(IV) oxide; In dichloromethane; at 20℃; for 54h; | 149 g (1714 mmol) of manganese dioxide is added in measured quantities to 28.0 g (148.9 mmol) of 2-bromo-4-hydroxymethyl-pyridine in 500 ml of dichloromethane within 6 hours. Then, stirring is continued at room temperature for 48 hours. It is suctioned off over Celite and concentrated by evaporation. 16.4 g of solidifying white oil accumulates. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
90% | With sodium tetrahydroborate; In methanol; at 0 - 20℃; for 1h;Inert atmosphere; | To a solution of <strong>[118289-17-1]2-bromopyridine-4-carbaldehyde</strong> (20 g, 107.52 mmol) in MeOH (150 mL) was added portion wise sodium borohydride (12.0 g, 322.56 mmol) at 0° C. under inert atmosphere. The mixture was stirred at RT for 1 h. Saturated NH4Cl solution was added followed by extraction with EtOAc (3*200 mL). The combined organic layers were dried (Na2SO4) and evaporated in vacuo to obtain i (18.0 g, 90percent). 1H NMR (DMSO-d6, 400 MHz): delta 8.30 (d, J=4.8 Hz, 1H), 7.54 (s, 1H), 7.35 (d, J=4.8 Hz, 1H), 5.55 (t, J=6.0 Hz, 1H) and 4.53-4.54 (d, J=5.6 Hz, 2H). |
With sodium tetrahydroborate; In methanol; at 0 - 25℃;Inert atmosphere; | In a flame dried round-bottomed flask equipped with a magnetic stir bar and under inert atmosphere (N2), <strong>[118289-17-1]2-bromo-pyridine-4-carbaldehyde</strong> (904 mg, 4.86 mmol) was dissolved in MeOH (10 mL). NaBH4 (236 mg, 5.99 mmol) was added portionwise at 0 0C and the reaction mixture stirred at rt for 1 h. Water (10 mL) was added and the mixture extracted <n="85"/>with EA (3 x 20 ml_). The combined org. extracts were dried over Na2SO4, filtered, and the solvents were removed under reduced pressure to give the title compound as a white solid. TLC: rf (1 :1 hept-EA) = 0.22. LC-MS-conditions 02: tR = 0.63 min; [M+H]+ = 188.33. |
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