ChemicalBook CAS DataBase List 2,2'-Bipyridine

2,2'-Bipyridine synthesis

11synthesis methods

Product Name:2,2'-Bipyridine
CAS Number:366-18-7
Molecular formula:C10H8N2
Molecular Weight:156.18

2,2'-bipyridine is synthesized by the reaction of pyridine with ferric chloride. Take 70g of anhydrous pyridine and mix with 13g of anhydrous ferric chloride, heat and react at 300℃ in a sealed tube for about 35h. After cooling, the reactant solidified into red-black crystals, the sealing tube was opened, and the red-black solution of the solid was washed out with a small amount of hot water. The oily impurities were removed by extraction with ether. After neutralization with sodium bicarbonate, excess pyridine was removed by heating with steam. The mixture was then made strongly basic, and the 2,2'-bipyridine was distilled off with steam.

29745-44-6
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109-73-9 Synthesis

109-73-9
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366-18-7
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Yield:366-18-7 96.7%

Reaction Conditions:

with dmap;copper(II) ethylacetoacetate;C₂₆H₃₆NP;silver(I) acetate in 1,2-dichloro-ethane at 90; for 8 h;Reagent/catalyst;

Steps:

3 Example 3: 2,2'-bipyridyl

At room temperature, the reactor proper amount of 1,2-dichloroethane, was added pyridine-2-carboxylic acid chloride 100mmol, 200mmol n-butylamine, 15mmol copper(II) ethylacetoacetate, 10mmol ligands L1,200mmol dimethylaminopyridine and 60mmol silver acetate, stirring heated to 90 , and the temperatureThe reaction was continued for 8 hours with stirring. TheAfter the completion of the reaction, the reaction system was allowed to cool to room temperature and washed thoroughly with deionized water. The organic layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure. The resulting residue was subjected to silica gel column chromatography, The mixture of n-butanol and ethyl acetate in a volume ratio of 1: 5 gave the compound of formula (I) 2,2'-bipyridine in a yield of 96.7%.

References:

CN104529879,2016,B Location in patent:Paragraph 0058; 0059; 0060; 0061; 0062; 0063

5029-67-4 Synthesis