3-(4-CHLORO-PHENYL)-PYRIDINE synthesis

13synthesis methods

Product Name:3-(4-CHLORO-PHENYL)-PYRIDINE
CAS Number:5957-97-1
Molecular formula:C11H8ClN
Molecular Weight:189.64

626-55-1 Synthesis

626-55-1
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$5.00/5/ G

1679-18-1 Synthesis

1679-18-1
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$10.00/1g

5957-97-1
22 suppliers
$355.00/1g

Yield:5957-97-1 100%

Reaction Conditions:

with tetrakis-(triphenylphosphine)-palladium;potassium carbonate in ethanol;lithium hydroxide monohydrate;toluene at 75; for 24 h;Inert atmosphere;Reflux;

Steps:

2.I

In other words, under nitrogen, to an 1L flask equipped witha stirrer& cooling tube, 3-Promo pyridine 11.5g (72.7mmol), 4- chlororphenyl boronacid 12.5g (79.9mmol), toluene 200mL, ethanol 100 mL and 2M aqueous solution ofpotassium carbonate 145mL were put and nitrogen bubbling was done for 7 minuteswhile stirring.There to, Pd (PPh₃)₄, 842mg (0.727mmol) was added and themixture was refluxed for 24 hours at a liquid temperature of 75 . After cooling, the separated lowermost layer in 3 layers was removedby liquid separation, the upper layer was washed twice with 5% brine 140mL by liquid separation. The resulting organic layer was dried with sodiumsulfate, and sodium sulfate was removed by filtration and evaporated. To givean oil 16.2g of turret yellow color. The resulting oil was purified by silicagel column chromatography (silica gel 200 g, ethyl acetate / hexane = 1/1) togive the compound 1 of 14.2 g. The yield was 100%. Compound 1 was a yellow oil.

References:

JP2015/214512,2015,A Location in patent:Paragraph 0034-0036

1120-90-7 Synthesis