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ChemicalBook CAS DataBase List 3-(4-BROMOPHENYL)PYRIDINE

3-(4-BROMOPHENYL)PYRIDINE synthesis

10synthesis methods
-

Yield:129013-83-8 92%

Reaction Conditions:

with tetrakis-(triphenylphosphine)-palladium;anhydrous sodium carbonate in ethanol;water monomer;toluene; for 1.5 h;Inert atmosphere;Reflux;

Steps:

6.1 first step

In a 1000 ml reaction flask, with mechanical stirring, Ar gas protection, adding 10. 01g (molecular weight 282,0 · 0355 mol), pyridine -3-boric acid 4 · 37 g (molecular weight 123, 0.0355 mol), catalyst Pd (PPh3) 4 dosage 2 · 14g (molecular weight 1154, 0.00185mol), sodium carbonate aqueous solution 200ml (2M), toluene 200ml, ethyl 200ml. The mixture was stirred under reflux and the reaction was monitored by TLC. After 1.5 hrs of reaction, the plate was found and the reaction was found to be complete. It was cooled, extracted with ethyl acetate, evaporated to dryness and purified by column chromatography. The eluent was petroleum ether: ethyl acetate = 20:1 (V1/V2), yielding white solid 7.73 g, molecular weight 232, HPLC at 98.1% yield: 92.0%

References:

CN104513206,2019,B Location in patent:Paragraph 0082-0086

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