4,4'-Dimethyl-2,2'-bipyridyl synthesis
- Product Name:4,4'-Dimethyl-2,2'-bipyridyl
- CAS Number:1134-35-6
- Molecular formula:C12H12N2
- Molecular Weight:184.24
1003-67-4
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1134-35-6
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Yield:1134-35-6 97.4%
Reaction Conditions:
Stage #1:4-methylpyridine-1-oxide with palladium on activated charcoal at 65; for 6 h;
Stage #2: with phosphorus trichlorideCatalytic behavior;Temperature;
Steps:
6
0.93 g of analytically pure 4-methylpyridine was weighed, added to the reaction flask, then add 20mL acetic acid dissolved raw materials, 15 mL of hydrogen peroxide at a mass concentration of 30% was added in two portions, and allowed to stand at room temperature to oxidize 4-methylpyridine. After 3.5 hours, 0.0118 g palladium on carbon catalyst was added, under an oil bath at 65 °C, heating reflux reaction. After about 6 h, stop the reaction. After the reaction solution was cooled to room temperature, adding 165 g of phosphorus trichloride to deoxygenation, and then use the Buchner funnel on the reaction bottle liquid decompression pumping operation, filter insoluble matter. The filtrate was evaporated under reduced pressure to remove the solvent, the resulting residue was white crystals. The white crystals were recrystallized from 20 mL of ethyl acetate. The resulting crystals were dried in vacuo and the yield of the obtained 4,4'-dimethyl-2,2'-bipyridine was 0.8972 g, and the yield was 97.4%.
References:
Henan Normal University;Guo Zhijun;Zhang Weiwei;Guo Libing;Li Yujiang;Xu Xia CN104892494, 2017, B Location in patent:Paragraph 0023-0024
4926-28-7
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1134-35-6
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108-89-4
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1134-35-6
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3678-62-4
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1134-35-6
289 suppliers
$5.00/1g