3-(5-BROMOPYRIDIN-3-YL)PYRIDINE synthesis
- Product Name:3-(5-BROMOPYRIDIN-3-YL)PYRIDINE
- CAS Number:15862-22-3
- Molecular formula:C10H7BrN2
- Molecular Weight:235.08
Yield:15862-22-3 75%
Reaction Conditions:
with tetrakis(triphenylphosphine) palladium(0);potassium carbonate in ethanol;toluene at 80; for 12 h;Inert atmosphere;
Steps:
1 (1) Synthesis of Intermediate 1
In a 100 mL two-necked flask, pyridine-3-boronic acid (246 mg, 1 mmol), bromopyridine (434 mg, 1 mmol), toluene (, ethanol, potassium carbonate aqueous solution (1.5 mL, 3 mmol), and tetrakis (triphenyl) were placed under a nitrogen atmosphere. Palladium (57 mg, 0.05 mmol) was refluxed for 12 hours at 80 ° C. After completion of the reaction, cooled to room temperature and filtered.The filtrate was diluted with 18 mL of deionized water, and the organic layer was separated.The aqueous layer was extracted with dichloromethane (3×18 mL). After combining the organic phases,It was dried over anhydrous magnesium sulfate and filtered, and the filtrate was evaporated under reduced pressure to remove solvent.The crude product obtained is purified by a mixture of petroleum ether and ethyl acetate in a 7:1 (v:v) mixture.1 as a white solid.
References:
CN108503625,2018,A Location in patent:Paragraph 0028; 0030-0033
