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CAS No. : | 118289-17-1 | MDL No. : | MFCD04039311 |
Formula : | C6H4BrNO | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | RTWLIQFKXMWEJY-UHFFFAOYSA-N |
M.W : | 186.01 | Pubchem ID : | 2762991 |
Synonyms : |
|
Chemical Name : | 2-Bromopyridine-4-carboxaldehyde |
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 |
---|---|---|
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 |
---|---|---|
64% | (3) To a solution of 2.91g of the compound obtained in the above (2) in 9mL of tetrahydrofuran was added dropwise 6.25mL of 1.6M n-butyl lithium-hexan solution under a nitrogen atmosphere under dry ice-acetone cooled condition, and the mixture was stirred at the same temperature for 30 minutes. To the reaction solution was added dropwise a solution of 1.86g of 2-bromo-4-formylpyridine in 9mL of tetrahydrofuran, and the mixture was stirred for 1 hour. To the reaction solution was added 30mL of saturated aqueous ammonium chloride solution, and the solution was extracted with 30mL of ethyl acetate. The aqueous layer was extracted with 30mL of ethyl acetate again, and the extracts were combined and washed with saturated saline, then dried over magnesium sulfate, and concentrated under reduced pressure. The residue was triturated with 100mL of chloroform and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel (solvent; n-hexan/ethyl acetate=3/1 to 1/1) to give 2.53g of 3,4-dimethoxy-6-(2-bromo-4-pyridyl)(hydroxy)methylbenzaldehyde dimethylacetal (yield: 64percent). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Synthesis of intermediate H-b: 2-Bromo-pyridine-4-carbaldehydeTo a suspension of Il-a (10.5 g, 52.23 mmol) in water (50 mL) were added successively dropwise at -10°C concentrated solution of HC1 (50 mL) and a solution of formaldehyde (50 mL) in water (37percent w/w). The reaction mixture was stirred at -10°C for 4 h. Then, a solution of NaOH (2 N) was added until pH = 6-7. The crude product was extracted with EtOAc (2 times) and the organic layer was washed with water, then with a saturated solution of NaCl, dried over MgS04 and concentrated to give Il-b as brownish oil in 97 percent yield. ? NMR (300 MHz, DMSO- 6) delta 10.03 (s, 1H), 8.68 (d, J = 4.9 Hz, 1H), 8.07 (s, 1H), 7.84 (d, J= 4.9 Hz, 1H). |
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