4,4'-Bis(methoxycarbonly)-2,2'-bipyridine synthesis
- Product Name:4,4'-Bis(methoxycarbonly)-2,2'-bipyridine
- CAS Number:71071-46-0
- Molecular formula:C14H12N2O4
- Molecular Weight:272.26
366-18-7
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79-22-1
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71071-46-0
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$11.00/250mg
Yield:71071-46-0 98.2%
Reaction Conditions:
with phosphotungstic acid;sodium tungstate;titanium(IV) oxide;zirconium(IV) oxide;triethylamine in methanol at 90; under 22502.3 Torr; for 5 h;Inert atmosphere;Solvent;Temperature;Pressure;
Steps:
1
The 2,2 '-bipyridine, methyl chloroformate, diethylamine, methanol and catalyst were mixed , then passes nitrogen gas and the reaction was carried out at 90 ° C at 3 MPa for 5 hours. In step 1), the molar ratio of 2,2 '-bipyridine, methyl chloroformate, triethylamine is 1: 2: 5; dose ratio of 2,2 '-bipyridine, methanol and catalyst is 1mol: 500ml: 0.3g;the mentioned catalyst was prepared by the following method: The phosphotungstic acid and sodium tungstate were dissolved in water and added a mixture of nanometer titanium dioxide and nano zirconia which is 6 times the weight of phosphotungstic acid (this mixture contained 70% by weight of titanium dioxide), stirred the reaction at 60 ° C for 30 h, then vacuum dried the moisture , an dried at 160 ° C for 2h; The mass ratio of the phosphotungstic acid, sodium tungstate and water is 1: 0.15: 5;after completion of the reaction, the mixture was filtered to remove insoluble matter, added to water, and extracted with ethyl acetate. After concentration, the product was obtained as a white solid 2,2'-bipyridinyl-4,4'-carboxylic acid methyl ester in a yield of 98.2%.
References:
Henan Business Ye Sciences Institute Co., Ltd.;Zhang Lipan;Wang Yong;Wang Fayun;Liu Hongwei;Guan Bingfeng;Guo Qingzhao;Zhang Yaxun;Ren Zhao CN106946772, 2017, A Location in patent:Paragraph 0017
67-56-1
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6813-38-3
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71071-46-0
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1134-35-6
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71071-46-0
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108-89-4
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71071-46-0
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695-34-1
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71071-46-0
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$11.00/250mg