Synthetic method for 2,2'-bipyridine-4,4'-methyl formate
A technique for the synthesis of methyl formate, applied in the direction of organic chemistry, can solve the problems of low total yield, dangerous operation, equipment corrosion, etc., and achieve the effect of high yield, cheap price and less pollution
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Embodiment 1
[0023] A method for synthesizing 2,2'-bipyridine-4,4'-methyl carboxylate, comprising the following steps:
[0024] 1) Mix 2,2'-bipyridine, methyl chloroformate, diethylamine, methanol and catalyst, blow nitrogen gas, and react at 90°C and 3 MPa for 5 hours; in step 1), 2,2'-bipyridine The molar ratio of pyridine, methyl chloroformate, and triethylamine is 1:2:5; the dosage ratio of 2,2'-bipyridyl, methanol, and catalyst is 1mol:500ml:0.3g;
[0025] The catalyst is prepared by the following method: dissolving phosphotungstic acid and sodium tungstate in water, adding a mixture of nano-titanium dioxide and nano-zirconia that is 6 times the weight of phosphotungstic acid (the mixture contains 70% by weight of titanium dioxide), Stir at 60°C for 30 hours, vacuum dry the water, and dry at 160°C for 2 hours; the mass ratio of phosphotungstic acid, sodium tungstate and water is 1:0.15:5;
[0026] 2) Cool after the reaction, filter to remove insoluble matter, add water, and then extr...
Embodiment 2
[0028] A method for synthesizing 2,2'-bipyridine-4,4'-methyl carboxylate, comprising the following steps:
[0029] 1) Mix 2,2'-bipyridine, methyl chloroformate, triethylamine, tetrahydrofuran and the catalyst described in Example 3, blow in argon, and react at 120°C and 4 MPa for 8 h; step 1) , the molar ratio of 2,2'-bipyridine, methyl chloroformate, and triethylamine is 1:3.6:5.15; the ratio of 2,2'-bipyridine, tetrahydrofuran, and catalyst is 1mol:700ml:0.6g;
[0030] The catalyst is prepared by the following method: dissolve phosphotungstic acid and sodium tungstate in water, the mass ratio of phosphotungstic acid, sodium tungstate and water is 1:0.20:6; then add phosphotungstic acid weight 7 times the mixture of nano-titanium dioxide and nano-zirconia (the mixture contains 66% by weight of titanium dioxide), stirred at 55 ° C for 28 h, vacuumed to dry the water, and dried at 160 ° C for 2 h to obtain the catalyst;
[0031] 2) After the reaction is finished, cool, filter ...
Embodiment 3
[0033] A method for synthesizing 2,2'-bipyridine-4,4'-methyl carboxylate, comprising the following steps:
[0034] 1) Mix 2,2'-bipyridine, methyl chloroformate, ethylenediamine, chloroform and the catalyst described in Example 2, blow nitrogen gas, and react at 100°C and 3.5 MPa for 9 h; in step 1), The molar ratio of 2,2'-bipyridine, methyl chloroformate, and triethylamine is 1:3:5.1; the molar ratio of 2,2'-bipyridine, tetrahydrofuran, and catalyst is 1mol:800ml:0.8g;
[0035] The catalyst is prepared by the following method: dissolve phosphotungstic acid and sodium tungstate in water, the mass ratio of phosphotungstic acid, sodium tungstate and water is 1:0.26:8; then add phosphotungstic acid weight 8 times the mixture of nano-titanium dioxide and nano-zirconia (the mixture contains 60% by weight of titanium dioxide), stirred at 45°C for 40h, vacuum-dried the water, and dried at 120°C for 5h to obtain the catalyst;
[0036] 2) Cool down after the reaction, filter to remove...
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